#------------------------------------------------------------------------------
#$Date: 2021-09-06 13:00:09 +0200 (lun 06 de sep de 2021) $
#$Revision: 268727 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/76/7707641.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7707641
loop_
_publ_author_name
'Mevissen, Christian'
'Sommer, David'
'Vasanthakumar, Sabarina'
'Truong, Khai-Nghi'
'Rissanen, Kari'
'Albrecht, Markus'
_publ_section_title
;
 Cation-translocation based isomerism offers a tool for the expansion of
 compressed helicates.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9372
_journal_page_last               9375
_journal_paper_doi               10.1039/d1dt01707a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C72 H81 Li3 Na O37.50 Ti2, 2(C3 H7 N O), H O0.50'
_chemical_formula_sum            'C78 H96 Li3 N2 Na O40 Ti2'
_chemical_formula_weight         1841.17
_chemical_name_systematic        Na[Li3(1)3Ti2]
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-03-11 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6785(2)
_cell_length_b                   40.9426(5)
_cell_length_c                   14.4762(2)
_cell_measurement_reflns_used    23814
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.9030
_cell_measurement_theta_min      3.3000
_cell_volume                     8283.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            77475
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration 
over a multifaceted crystal model.
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 4286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.094(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         15371
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0821P)²+4.0271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                12018
_reflns_number_total             15371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01707a2.cif
_cod_data_source_block           Na[Li3(1)3Ti2]
_cod_depositor_comments
'Adding full bibliography for 7707641--7707642.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7707641
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.905
_oxdiff_exptl_absorpt_empirical_full_min 0.815
_oxdiff_exptl_absorpt_empirical_full_max 1.251
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.41602(10) 0.65447(3) 0.27768(9) 0.0323(3) Uani 1 1 d . . . . .
Ti2 Ti 0.63118(10) 0.66411(3) 0.66067(9) 0.0315(3) Uani 1 1 d . . . . .
Na1 Na 0.0109(8) 0.56406(17) 0.4867(6) 0.138(3) Uani 1 1 d . . . . .
Li1 Li 0.4176(9) 0.6363(3) 0.5080(9) 0.031(2) Uani 1 1 d . . . . .
Li2 Li 0.6351(10) 0.6361(3) 0.4399(10) 0.037(3) Uani 1 1 d . . . . .
Li3 Li 0.5116(11) 0.7103(3) 0.4602(10) 0.035(3) Uani 1 1 d . . . . .
O1 O 0.3126(4) 0.68305(14) 0.2197(4) 0.0391(12) Uani 1 1 d . . . . .
O2 O 0.3648(4) 0.66122(12) 0.3910(4) 0.0310(11) Uani 1 1 d . . . . .
O3 O 0.3239(4) 0.65450(13) 0.5661(4) 0.0374(12) Uani 1 1 d . . . . .
O4 O 0.1940(4) 0.68123(15) 0.5763(4) 0.0435(14) Uani 1 1 d . . . . .
O5 O 0.0620(5) 0.64566(16) 0.6530(5) 0.0532(16) Uani 1 1 d . . . . .
O6 O -0.0333(8) 0.5862(2) 0.6294(9) 0.104(3) Uani 1 1 d . . . . .
O7 O 0.0775(9) 0.5293(2) 0.6402(10) 0.108(3) Uani 1 1 d . . . . .
O8 O 0.2499(9) 0.4930(3) 0.5506(10) 0.117(3) Uani 1 1 d D . . . .
O9 O 0.3955(7) 0.53636(18) 0.5203(7) 0.087(3) Uani 1 1 d . . . . .
O10 O 0.3855(5) 0.59042(14) 0.4928(5) 0.0485(14) Uani 1 1 d . . . . .
O11 O 0.5461(4) 0.62688(12) 0.5930(4) 0.0353(12) Uani 1 1 d . . . . .
O12 O 0.7033(4) 0.62800(13) 0.7274(4) 0.0403(13) Uani 1 1 d . . . . .
O13 O 0.4742(4) 0.66036(13) 0.1772(4) 0.0375(12) Uani 1 1 d . . . . .
O14 O 0.5155(4) 0.68852(12) 0.3400(3) 0.0301(11) Uani 1 1 d . . . . .
O15 O 0.6107(4) 0.74052(13) 0.4551(4) 0.0372(12) Uani 1 1 d . . . . .
O16 O 0.7086(4) 0.76963(14) 0.3963(4) 0.0398(13) Uani 1 1 d . . . . .
O17 O 0.7611(7) 0.83632(19) 0.4221(6) 0.077(2) Uani 1 1 d . . . . .
O18 O 0.6712(11) 0.8974(3) 0.4128(11) 0.132(4) Uani 1 1 d . . . . .
O19 O 0.5388(9) 0.8768(4) 0.5085(11) 0.141(5) Uani 1 1 d . . . . .
O20 O 0.3784(6) 0.8341(2) 0.4916(5) 0.075(2) Uani 1 1 d . . . . .
O21 O 0.3128(5) 0.77065(16) 0.5162(4) 0.0569(19) Uani 1 1 d . . . . .
O22 O 0.4122(4) 0.74120(12) 0.4598(3) 0.0338(11) Uani 1 1 d . . . . .
O23 O 0.5221(4) 0.69407(12) 0.5890(3) 0.0289(10) Uani 1 1 d . . . . .
O24 O 0.5759(4) 0.67261(13) 0.7616(4) 0.0352(12) Uani 1 1 d . . . . .
O25 O 0.3546(4) 0.61454(14) 0.2256(4) 0.0426(13) Uani 1 1 d . . . . .
O26 O 0.5095(4) 0.62143(12) 0.3602(4) 0.0340(12) Uani 1 1 d . . . . .
O27 O 0.6775(5) 0.59222(14) 0.4721(4) 0.0446(14) Uani 1 1 d . . . . .
O28 O 0.6786(7) 0.53773(16) 0.4743(6) 0.080(3) Uani 1 1 d . . . . .
O29 O 0.8579(16) 0.5200(4) 0.4404(18) 0.190(7) Uani 1 1 d D . . . .
O30 O 0.9795(10) 0.5244(4) 0.3387(12) 0.147(6) Uani 1 1 d D . . . .
O31 O 1.0749(9) 0.5802(2) 0.3422(9) 0.110(3) Uani 1 1 d . . . . .
O32 O 0.9768(5) 0.64044(16) 0.2899(5) 0.0534(16) Uani 1 1 d . . . . .
O33 O 0.8443(5) 0.68072(18) 0.3507(4) 0.0542(17) Uani 1 1 d . . . . .
O34 O 0.7251(4) 0.65233(13) 0.3758(4) 0.0375(12) Uani 1 1 d . . . . .
O35 O 0.6803(4) 0.66722(12) 0.5455(4) 0.0299(11) Uani 1 1 d . . . . .
O36 O 0.7289(4) 0.69566(13) 0.7063(4) 0.0367(12) Uani 1 1 d . . . . .
O37 O -0.1194(17) 0.5957(3) 0.3888(13) 0.091(5) Uani 0.5 1 d . . P . .
H37O H -0.091441 0.608369 0.360734 0.109 Uiso 0.5 1 d R U P . .
H37P H -0.160249 0.610383 0.385716 0.109 Uiso 0.5 1 d R U P . .
O38 O 0.1503(10) 0.5949(3) 0.5643(9) 0.1150(19) Uani 1 1 d . . . . .
H38O H 0.126086 0.609526 0.590166 0.138 Uiso 1 1 d R U . . .
H38P H 0.204541 0.591241 0.603772 0.138 Uiso 1 1 d R U . . .
C1 C 0.2864(6) 0.68015(18) 0.3701(6) 0.0351(16) Uani 1 1 d . . . . .
C2 C 0.2590(6) 0.69328(19) 0.2751(6) 0.0365(17) Uani 1 1 d . . . . .
C3 C 0.1828(6) 0.7145(2) 0.2433(6) 0.0430(19) Uani 1 1 d . . . . .
H3 H 0.166480 0.723803 0.180282 0.052 Uiso 1 1 calc R U . . .
C4 C 0.1298(7) 0.7219(2) 0.3069(7) 0.048(2) Uani 1 1 d . . . . .
H4 H 0.077331 0.736527 0.286680 0.057 Uiso 1 1 calc R U . . .
C5 C 0.1530(6) 0.7082(2) 0.3976(6) 0.0404(18) Uani 1 1 d . . . . .
H5 H 0.114756 0.713092 0.438244 0.048 Uiso 1 1 calc R U . . .
C6 C 0.2315(6) 0.68713(18) 0.4321(6) 0.0335(16) Uani 1 1 d . . . . .
C7 C 0.2564(6) 0.67265(19) 0.5299(6) 0.0363(17) Uani 1 1 d . . . . .
C8 C 0.2145(7) 0.6698(3) 0.6754(6) 0.050(2) Uani 1 1 d . . . . .
H8A H 0.263515 0.683812 0.719951 0.060 Uiso 1 1 calc R U . . .
H8B H 0.238958 0.647086 0.681125 0.060 Uiso 1 1 calc R U . . .
C9 C 0.1227(7) 0.6712(3) 0.7006(7) 0.053(2) Uani 1 1 d . . . . .
H9A H 0.136256 0.669071 0.771695 0.063 Uiso 1 1 calc R U . . .
H9B H 0.090948 0.692519 0.680372 0.063 Uiso 1 1 calc R U . . .
C10 C -0.0147(7) 0.6405(3) 0.6929(9) 0.061(3) Uani 1 1 d . . . . .
H10A H -0.049963 0.661144 0.691435 0.073 Uiso 1 1 calc R U . . .
H10B H 0.011483 0.633386 0.761299 0.073 Uiso 1 1 calc R U . . .
C11 C -0.0811(10) 0.6151(3) 0.6362(13) 0.092(4) Uani 1 1 d . . . . .
H11A H -0.130799 0.610448 0.667815 0.111 Uiso 1 1 calc R U . . .
H11B H -0.113537 0.623453 0.570194 0.111 Uiso 1 1 calc R U . . .
C12 C -0.0019(12) 0.5689(3) 0.7099(12) 0.087(4) Uani 1 1 d . . . . .
H12A H -0.053102 0.553529 0.712767 0.105 Uiso 1 1 calc R U . . .
H12B H 0.009380 0.583895 0.765858 0.105 Uiso 1 1 calc R U . . .
C13 C 0.0860(17) 0.5500(7) 0.721(2) 0.169(6) Uani 1 1 d . . . . .
H13A H 0.140187 0.565244 0.728522 0.203 Uiso 1 1 calc R U . . .
H13B H 0.100100 0.536592 0.780686 0.203 Uiso 1 1 calc R U . . .
C14 C 0.1638(17) 0.5149(7) 0.6430(18) 0.169(6) Uani 1 1 d D . . . .
H14A H 0.174343 0.494900 0.683193 0.203 Uiso 1 1 calc R U . . .
H14B H 0.217398 0.530196 0.671213 0.203 Uiso 1 1 calc R U . . .
C15 C 0.1578(15) 0.5067(7) 0.5399(18) 0.169(6) Uani 1 1 d D . . . .
H15A H 0.106288 0.490688 0.511623 0.203 Uiso 1 1 calc R U . . .
H15B H 0.146741 0.526489 0.498650 0.203 Uiso 1 1 calc R U . . .
C16 C 0.2687(13) 0.5031(4) 0.4720(15) 0.117(3) Uani 1 1 d D . . . .
H16A H 0.206640 0.501543 0.420211 0.141 Uiso 1 1 calc R U . . .
H16B H 0.309157 0.485603 0.457996 0.141 Uiso 1 1 calc R U . . .
C17 C 0.3102(13) 0.5326(4) 0.4511(16) 0.117(3) Uani 1 1 d D . . . .
H17A H 0.319310 0.531235 0.386164 0.141 Uiso 1 1 calc R U . . .
H17B H 0.267893 0.551348 0.451619 0.141 Uiso 1 1 calc R U . . .
C18 C 0.4300(8) 0.5671(2) 0.5351(7) 0.055(2) Uani 1 1 d . . . . .
C19 C 0.5237(7) 0.5686(2) 0.6101(7) 0.049(2) Uani 1 1 d . . . . .
C20 C 0.5729(7) 0.59774(19) 0.6340(6) 0.0428(19) Uani 1 1 d . . . . .
C21 C 0.6622(7) 0.5987(2) 0.7100(7) 0.047(2) Uani 1 1 d . . . . .
C22 C 0.7003(8) 0.5709(2) 0.7608(8) 0.057(2) Uani 1 1 d . . . . .
H22 H 0.759779 0.571659 0.810874 0.069 Uiso 1 1 calc R U . . .
C23 C 0.6495(9) 0.5417(3) 0.7370(9) 0.070(3) Uani 1 1 d . . . . .
H23 H 0.674773 0.522505 0.772339 0.084 Uiso 1 1 calc R U . . .
C24 C 0.5642(9) 0.5400(3) 0.6639(9) 0.065(3) Uani 1 1 d . . . . .
H24 H 0.531725 0.519650 0.648959 0.078 Uiso 1 1 calc R U . . .
C25 C 0.5573(6) 0.70210(18) 0.2784(5) 0.0323(16) Uani 1 1 d . . . . .
C26 C 0.5329(6) 0.68573(19) 0.1869(5) 0.0337(16) Uani 1 1 d . . . . .
C27 C 0.5704(6) 0.6960(2) 0.1152(5) 0.0361(16) Uani 1 1 d . . . . .
H27 H 0.554343 0.684921 0.054708 0.043 Uiso 1 1 calc R U . . .
C28 C 0.6330(7) 0.7232(2) 0.1328(6) 0.045(2) Uani 1 1 d . . . . .
H28 H 0.659523 0.730415 0.084139 0.053 Uiso 1 1 calc R U . . .
C29 C 0.6556(6) 0.7393(2) 0.2217(6) 0.0396(17) Uani 1 1 d . . . . .
H29 H 0.696655 0.757771 0.232565 0.047 Uiso 1 1 calc R U . . .
C30 C 0.6190(5) 0.72871(18) 0.2958(5) 0.0313(15) Uani 1 1 d . . . . .
C31 C 0.6437(6) 0.74615(18) 0.3894(5) 0.0333(16) Uani 1 1 d . . . . .
C32 C 0.7386(7) 0.7861(2) 0.4895(5) 0.0432(19) Uani 1 1 d . . . . .
H32A H 0.767193 0.770323 0.542062 0.052 Uiso 1 1 calc R U . . .
H32B H 0.683051 0.796656 0.502560 0.052 Uiso 1 1 calc R U . . .
C33 C 0.8103(7) 0.8111(3) 0.4848(6) 0.055(3) Uani 1 1 d . . . . .
H33A H 0.842335 0.820045 0.550315 0.066 Uiso 1 1 calc R U . . .
H33B H 0.859600 0.801338 0.459517 0.066 Uiso 1 1 calc R U . . .
C34 C 0.8160(13) 0.8652(4) 0.4387(15) 0.119(4) Uani 1 1 d D . . . .
H34A H 0.841829 0.869659 0.509124 0.142 Uiso 1 1 calc R U . . .
H34B H 0.870245 0.863149 0.411873 0.142 Uiso 1 1 calc R U . . .
C35 C 0.7535(13) 0.8909(4) 0.3911(16) 0.119(4) Uani 1 1 d D . . . .
H35A H 0.791646 0.911265 0.402373 0.142 Uiso 1 1 calc R U . . .
H35B H 0.735153 0.886406 0.320569 0.142 Uiso 1 1 calc R U . . .
C36 C 0.6667(13) 0.9096(5) 0.4921(12) 0.108(3) Uani 1 1 d D . . . .
H36A H 0.622939 0.928563 0.477114 0.129 Uiso 1 1 calc R U . . .
H36B H 0.730961 0.917677 0.529276 0.129 Uiso 1 1 calc R U . . .
C37 C 0.6358(15) 0.8883(6) 0.5499(15) 0.147(8) Uani 1 1 d D . . . .
H37A H 0.641000 0.899280 0.612255 0.176 Uiso 1 1 calc R U . . .
H37B H 0.679122 0.869164 0.564364 0.176 Uiso 1 1 calc R U . . .
C38 C 0.5306(15) 0.8433(5) 0.4709(15) 0.108(3) Uani 1 1 d . . . . .
H38A H 0.569277 0.840991 0.426011 0.129 Uiso 1 1 calc R U . . .
H38B H 0.556221 0.827870 0.525450 0.129 Uiso 1 1 calc R U . . .
C39 C 0.4307(12) 0.8349(5) 0.4197(12) 0.108(3) Uani 1 1 d . . . . .
H39A H 0.427203 0.813285 0.388082 0.129 Uiso 1 1 calc R U . . .
H39B H 0.402228 0.851381 0.369128 0.129 Uiso 1 1 calc R U . . .
C40 C 0.2785(8) 0.8236(2) 0.4485(6) 0.055(2) Uani 1 1 d . . . . .
H40A H 0.241873 0.827539 0.494657 0.066 Uiso 1 1 calc R U . . .
H40B H 0.248122 0.836174 0.388523 0.066 Uiso 1 1 calc R U . . .
C41 C 0.2788(9) 0.7889(2) 0.4264(6) 0.059(3) Uani 1 1 d . . . . .
H41A H 0.213339 0.781676 0.389802 0.071 Uiso 1 1 calc R U . . .
H41B H 0.321049 0.784773 0.385813 0.071 Uiso 1 1 calc R U . . .
C42 C 0.3811(6) 0.74829(18) 0.5258(5) 0.0350(16) Uani 1 1 d . . . . .
C43 C 0.4141(6) 0.73377(17) 0.6244(5) 0.0312(15) Uani 1 1 d . . . . .
C44 C 0.4795(5) 0.70901(17) 0.6488(5) 0.0280(14) Uani 1 1 d . . . . .
C45 C 0.5095(6) 0.69677(18) 0.7444(5) 0.0312(15) Uani 1 1 d . . . . .
C46 C 0.4722(6) 0.70868(19) 0.8143(5) 0.0356(16) Uani 1 1 d . . . . .
H46 H 0.491525 0.699918 0.878121 0.043 Uiso 1 1 calc R U . . .
C47 C 0.4056(6) 0.73378(19) 0.7891(6) 0.0367(17) Uani 1 1 d . . . . .
H47 H 0.379723 0.742431 0.836621 0.044 Uiso 1 1 calc R U . . .
C48 C 0.3763(6) 0.74637(18) 0.6966(5) 0.0346(16) Uani 1 1 d . . . . .
H48 H 0.330662 0.763556 0.680967 0.042 Uiso 1 1 calc R U . . .
C49 C 0.4882(7) 0.5906(2) 0.3317(6) 0.0407(18) Uani 1 1 d . . . . .
C50 C 0.4020(7) 0.58693(19) 0.2562(6) 0.0439(19) Uani 1 1 d . . . . .
C51 C 0.3733(9) 0.5564(2) 0.2177(8) 0.063(3) Uani 1 1 d . . . . .
H51 H 0.316436 0.554007 0.164715 0.076 Uiso 1 1 calc R U . . .
C52 C 0.4273(10) 0.5296(2) 0.2566(10) 0.079(4) Uani 1 1 d . . . . .
H52 H 0.404505 0.508569 0.233105 0.094 Uiso 1 1 calc R U . . .
C53 C 0.5131(10) 0.5322(3) 0.3282(9) 0.073(3) Uani 1 1 d . . . . .
H53 H 0.550227 0.513254 0.351473 0.088 Uiso 1 1 calc R U . . .
C54 C 0.5465(7) 0.5631(2) 0.3672(7) 0.051(2) Uani 1 1 d . . . . .
C55 C 0.6394(7) 0.5669(2) 0.4428(7) 0.049(2) Uani 1 1 d . . . . .
C56 C 0.7713(11) 0.5376(4) 0.5455(11) 0.092(4) Uani 1 1 d . . . . .
H56A H 0.764603 0.532465 0.609989 0.110 Uiso 1 1 calc R U . . .
H56B H 0.800510 0.559499 0.548979 0.110 Uiso 1 1 calc R U . . .
C57 C 0.835(2) 0.5127(6) 0.521(2) 0.164(6) Uani 1 1 d . . . . .
H57A H 0.895107 0.510845 0.575604 0.197 Uiso 1 1 calc R U . . .
H57B H 0.803259 0.491156 0.511952 0.197 Uiso 1 1 calc R U . . .
C58 C 0.897(2) 0.4900(5) 0.418(2) 0.164(6) Uani 1 1 d D . . . .
H58A H 0.957586 0.484536 0.468749 0.197 Uiso 1 1 calc R U . . .
H58B H 0.851240 0.471749 0.412370 0.197 Uiso 1 1 calc R U . . .
C59 C 0.9128(18) 0.4963(5) 0.3283(18) 0.157(6) Uani 1 1 d D . . . .
H59A H 0.851239 0.501411 0.278545 0.188 Uiso 1 1 calc R U . . .
H59B H 0.940414 0.476752 0.306875 0.188 Uiso 1 1 calc R U . . .
C60 C 0.978(2) 0.5380(6) 0.256(2) 0.157(6) Uani 1 1 d . . . . .
H60A H 0.916618 0.550155 0.230326 0.188 Uiso 1 1 calc R U . . .
H60B H 0.977281 0.520409 0.208575 0.188 Uiso 1 1 calc R U . . .
C61 C 1.0586(14) 0.5610(3) 0.2590(13) 0.110(3) Uani 1 1 d . . . . .
H61A H 1.116982 0.548450 0.261353 0.132 Uiso 1 1 calc R U . . .
H61B H 1.041749 0.574970 0.200429 0.132 Uiso 1 1 calc R U . . .
C62 C 1.1235(11) 0.6105(3) 0.3315(11) 0.089(3) Uani 1 1 d . . . . .
H62A H 1.178786 0.605238 0.308615 0.107 Uiso 1 1 calc R U . . .
H62B H 1.148237 0.621212 0.395650 0.107 Uiso 1 1 calc R U . . .
C63 C 1.0584(11) 0.6338(3) 0.2613(11) 0.089(3) Uani 1 1 d . . . . .
H63A H 1.092966 0.654392 0.259055 0.107 Uiso 1 1 calc R U . . .
H63B H 1.038606 0.624132 0.195439 0.107 Uiso 1 1 calc R U . . .
C64 C 0.9181(7) 0.6635(2) 0.2320(7) 0.049(2) Uani 1 1 d . . . . .
H64A H 0.905484 0.657816 0.162797 0.059 Uiso 1 1 calc R U . . .
H64B H 0.949097 0.685234 0.243577 0.059 Uiso 1 1 calc R U . . .
C65 C 0.8255(7) 0.6642(3) 0.2570(7) 0.055(2) Uani 1 1 d . . . . .
H65A H 0.775894 0.676156 0.206392 0.066 Uiso 1 1 calc R U . . .
H65B H 0.802505 0.641692 0.261094 0.066 Uiso 1 1 calc R U . . .
C66 C 0.7885(6) 0.6723(2) 0.4038(6) 0.0394(18) Uani 1 1 d . . . . .
C67 C 0.8123(6) 0.69008(19) 0.4967(6) 0.0368(17) Uani 1 1 d . . . . .
C68 C 0.7577(5) 0.68601(18) 0.5609(5) 0.0310(15) Uani 1 1 d . . . . .
C69 C 0.7855(6) 0.70238(18) 0.6507(6) 0.0342(16) Uani 1 1 d . . . . .
C70 C 0.8631(6) 0.7233(2) 0.6768(6) 0.0404(18) Uani 1 1 d . . . . .
H70 H 0.880717 0.734124 0.737739 0.048 Uiso 1 1 calc R U . . .
C71 C 0.9144(6) 0.7281(2) 0.6126(6) 0.0436(19) Uani 1 1 d . . . . .
H71 H 0.966394 0.743056 0.628584 0.052 Uiso 1 1 calc R U . . .
C72 C 0.8913(7) 0.7112(2) 0.5238(6) 0.0442(19) Uani 1 1 d . . . . .
H72 H 0.929327 0.714182 0.481870 0.053 Uiso 1 1 calc R U . . .
O39 O 0.3313(10) 0.5820(3) 0.7017(9) 0.1150(19) Uani 1 1 d . . . . .
N1 N 0.4692(13) 0.5879(4) 0.8358(12) 0.1150(19) Uani 1 1 d . . . . .
C73 C 0.4059(16) 0.5965(6) 0.7541(16) 0.132(7) Uani 1 1 d . . . . .
H73 H 0.417791 0.617033 0.729739 0.159 Uiso 1 1 calc R U . . .
C74 C 0.4653(15) 0.5569(4) 0.8804(13) 0.1150(19) Uani 1 1 d . . . . .
H74A H 0.409480 0.544674 0.841184 0.172 Uiso 1 1 calc R U . . .
H74B H 0.460029 0.560349 0.945586 0.172 Uiso 1 1 calc R U . . .
H74C H 0.523653 0.544554 0.884978 0.172 Uiso 1 1 calc R U . . .
C75 C 0.5469(15) 0.6099(4) 0.8844(13) 0.1150(19) Uani 1 1 d . . . . .
H75A H 0.541386 0.630056 0.846639 0.172 Uiso 1 1 calc R U . . .
H75B H 0.608357 0.599374 0.889985 0.172 Uiso 1 1 calc R U . . .
H75C H 0.543368 0.615057 0.949322 0.172 Uiso 1 1 calc R U . . .
O40 O 0.4270(18) 0.9279(6) 0.484(2) 0.133(10) Uani 0.5 1 d . . P . .
H40O H 0.461922 0.911227 0.491943 0.160 Uiso 0.5 1 d R U P . .
H40P H 0.380235 0.930286 0.504894 0.160 Uiso 0.5 1 d R U P . .
O41 O 0.2755(13) 0.9372(3) 0.5584(15) 0.166(7) Uani 1 1 d . . . . .
N2 N 0.1650(10) 0.9221(3) 0.6311(10) 0.096(4) Uani 1 1 d . . . . .
C76 C 0.2312(13) 0.9148(5) 0.5836(12) 0.110(6) Uani 1 1 d . . . . .
H76 H 0.242724 0.892724 0.570313 0.131 Uiso 1 1 calc R U . . .
C77 C 0.140(2) 0.9537(4) 0.646(2) 0.178(12) Uani 1 1 d . . . . .
H77A H 0.176383 0.960702 0.711855 0.267 Uiso 1 1 calc R U . . .
H77B H 0.071347 0.954656 0.638740 0.267 Uiso 1 1 calc R U . . .
H77C H 0.154298 0.968257 0.598662 0.267 Uiso 1 1 calc R U . . .
C78 C 0.1188(12) 0.8964(3) 0.6654(11) 0.087(4) Uani 1 1 d . . . . .
H78A H 0.050154 0.896745 0.630157 0.131 Uiso 1 1 calc R U . . .
H78B H 0.128214 0.899411 0.734877 0.131 Uiso 1 1 calc R U . . .
H78C H 0.145973 0.875419 0.654809 0.131 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O25 97.8(3) . . ?
O1 Ti1 O13 93.9(2) . . ?
O25 Ti1 O13 94.3(2) . . ?
O1 Ti1 O14 98.2(2) . . ?
O25 Ti1 O14 163.2(2) . . ?
O13 Ti1 O14 79.8(2) . . ?
O1 Ti1 O2 80.2(2) . . ?
O25 Ti1 O2 100.9(2) . . ?
O13 Ti1 O2 164.3(2) . . ?
O14 Ti1 O2 86.6(2) . . ?
O1 Ti1 O26 167.1(2) . . ?
O25 Ti1 O26 79.3(2) . . ?
O13 Ti1 O26 98.8(2) . . ?
O14 Ti1 O26 86.0(2) . . ?
O2 Ti1 O26 88.0(2) . . ?
O1 Ti1 Li1 109.4(3) . . ?
O25 Ti1 Li1 93.5(3) . . ?
O13 Ti1 Li1 154.1(3) . . ?
O14 Ti1 Li1 85.7(2) . . ?
O2 Ti1 Li1 29.4(2) . . ?
O26 Ti1 Li1 58.6(2) . . ?
O1 Ti1 Li2 153.2(3) . . ?
O25 Ti1 Li2 108.3(3) . . ?
O13 Ti1 Li2 90.3(3) . . ?
O14 Ti1 Li2 56.5(3) . . ?
O2 Ti1 Li2 88.7(3) . . ?
O26 Ti1 Li2 29.6(3) . . ?
Li1 Ti1 Li2 63.8(3) . . ?
O1 Ti1 Li3 90.7(3) . . ?
O25 Ti1 Li3 154.5(3) . . ?
O13 Ti1 Li3 109.1(3) . . ?
O14 Ti1 Li3 29.8(3) . . ?
O2 Ti1 Li3 56.8(3) . . ?
O26 Ti1 Li3 87.0(3) . . ?
Li1 Ti1 Li3 61.0(3) . . ?
Li2 Ti1 Li3 62.9(3) . . ?
O36 Ti2 O12 96.2(3) . . ?
O36 Ti2 O24 93.6(2) . . ?
O12 Ti2 O24 93.1(2) . . ?
O36 Ti2 O35 79.7(2) . . ?
O12 Ti2 O35 100.7(2) . . ?
O24 Ti2 O35 165.2(2) . . ?
O36 Ti2 O11 166.6(2) . . ?
O12 Ti2 O11 79.9(2) . . ?
O24 Ti2 O11 99.5(2) . . ?
O35 Ti2 O11 88.3(2) . . ?
O36 Ti2 O23 99.3(2) . . ?
O12 Ti2 O23 163.4(2) . . ?
O24 Ti2 O23 80.1(2) . . ?
O35 Ti2 O23 88.0(2) . . ?
O11 Ti2 O23 86.2(2) . . ?
O36 Ti2 Li2 109.1(3) . . ?
O12 Ti2 Li2 92.8(3) . . ?
O24 Ti2 Li2 155.7(3) . . ?
O35 Ti2 Li2 29.8(3) . . ?
O11 Ti2 Li2 58.5(3) . . ?
O23 Ti2 Li2 87.7(3) . . ?
O36 Ti2 Li1 153.7(3) . . ?
O12 Ti2 Li1 109.1(3) . . ?
O24 Ti2 Li1 92.0(3) . . ?
O35 Ti2 Li1 88.6(3) . . ?
O11 Ti2 Li1 29.7(2) . . ?
O23 Ti2 Li1 56.6(2) . . ?
Li2 Ti2 Li1 63.8(3) . . ?
O36 Ti2 Li3 93.2(3) . . ?
O12 Ti2 Li3 155.8(3) . . ?
O24 Ti2 Li3 108.5(3) . . ?
O35 Ti2 Li3 59.3(3) . . ?
O11 Ti2 Li3 85.8(3) . . ?
O23 Ti2 Li3 28.7(3) . . ?
Li2 Ti2 Li3 63.1(3) . . ?
Li1 Ti2 Li3 60.8(3) . . ?
O38 Na1 O37 114.2(6) . . ?
O38 Na1 O6 79.7(4) . . ?
O37 Na1 O6 86.0(5) . . ?
O38 Na1 O7 80.8(5) . . ?
O37 Na1 O7 147.1(7) . . ?
O6 Na1 O7 67.3(4) . . ?
O38 Na1 O30 128.9(6) . 1_455 ?
O37 Na1 O30 86.7(6) . 1_455 ?
O6 Na1 O30 150.7(6) . 1_455 ?
O7 Na1 O30 106.9(6) . 1_455 ?
O38 Na1 O31 77.1(4) . 1_455 ?
O37 Na1 O31 78.9(5) . 1_455 ?
O6 Na1 O31 143.9(4) . 1_455 ?
O7 Na1 O31 134.0(6) . 1_455 ?
O30 Na1 O31 61.3(5) 1_455 1_455 ?
O38 Na1 O29 165.7(7) . 1_455 ?
O37 Na1 O29 76.6(7) . 1_455 ?
O6 Na1 O29 92.3(6) . 1_455 ?
O7 Na1 O29 85.2(6) . 1_455 ?
O30 Na1 O29 58.4(5) 1_455 1_455 ?
O31 Na1 O29 115.3(6) 1_455 1_455 ?
O38 Na1 C15 81.6(7) . . ?
O37 Na1 C15 157.5(7) . . ?
O6 Na1 C15 113.6(6) . . ?
O7 Na1 C15 47.0(6) . . ?
O30 Na1 C15 70.8(6) 1_455 . ?
O31 Na1 C15 89.9(6) 1_455 . ?
O29 Na1 C15 91.0(7) 1_455 . ?
O38 Na1 H38O 18.2 . . ?
O37 Na1 H38O 102.2 . . ?
O6 Na1 H38O 64.0 . . ?
O7 Na1 H38O 83.7 . . ?
O30 Na1 H38O 145.3 1_455 . ?
O31 Na1 H38O 87.2 1_455 . ?
O29 Na1 H38O 156.2 1_455 . ?
C15 Na1 H38O 96.6 . . ?
O2 Li1 O10 113.3(7) . . ?
O2 Li1 O11 135.4(7) . . ?
O10 Li1 O11 92.0(6) . . ?
O2 Li1 O3 91.7(5) . . ?
O10 Li1 O3 103.8(6) . . ?
O11 Li1 O3 118.3(7) . . ?
O2 Li1 Ti1 31.1(3) . . ?
O10 Li1 Ti1 99.9(5) . . ?
O11 Li1 Ti1 112.1(5) . . ?
O3 Li1 Ti1 122.7(5) . . ?
O2 Li1 Ti2 115.7(5) . . ?
O10 Li1 Ti2 122.6(5) . . ?
O11 Li1 Ti2 30.9(3) . . ?
O3 Li1 Ti2 102.7(5) . . ?
Ti1 Li1 Ti2 106.8(3) . . ?
O2 Li1 Li3 56.1(4) . . ?
O10 Li1 Li3 156.9(6) . . ?
O11 Li1 Li3 86.1(5) . . ?
O3 Li1 Li3 97.3(5) . . ?
Ti1 Li1 Li3 60.1(3) . . ?
Ti2 Li1 Li3 60.0(3) . . ?
O27 Li2 O35 114.6(7) . . ?
O27 Li2 O26 91.9(6) . . ?
O35 Li2 O26 134.6(8) . . ?
O27 Li2 O34 102.6(7) . . ?
O35 Li2 O34 91.9(6) . . ?
O26 Li2 O34 118.7(7) . . ?
O27 Li2 Ti2 100.7(5) . . ?
O35 Li2 Ti2 31.0(3) . . ?
O26 Li2 Ti2 112.0(6) . . ?
O34 Li2 Ti2 122.7(6) . . ?
O27 Li2 Ti1 122.6(6) . . ?
O35 Li2 Ti1 114.7(6) . . ?
O26 Li2 Ti1 31.1(3) . . ?
O34 Li2 Ti1 103.2(5) . . ?
Ti2 Li2 Ti1 106.6(4) . . ?
O15 Li3 O22 99.1(6) . . ?
O15 Li3 O23 114.7(7) . . ?
O22 Li3 O23 93.8(6) . . ?
O15 Li3 O14 91.7(6) . . ?
O22 Li3 O14 121.3(8) . . ?
O23 Li3 O14 132.6(7) . . ?
O15 Li3 Ti1 122.0(6) . . ?
O22 Li3 Ti1 107.5(6) . . ?
O23 Li3 Ti1 113.7(5) . . ?
O14 Li3 Ti1 30.6(3) . . ?
O15 Li3 Ti2 100.8(6) . . ?
O22 Li3 Ti2 123.4(6) . . ?
O23 Li3 Ti2 30.2(3) . . ?
O14 Li3 Ti2 110.4(5) . . ?
Ti1 Li3 Ti2 105.2(3) . . ?
O15 Li3 Li1 156.1(7) . . ?
O22 Li3 Li1 103.0(6) . . ?
O23 Li3 Li1 55.3(4) . . ?
O14 Li3 Li1 84.4(5) . . ?
Ti1 Li3 Li1 58.9(3) . . ?
Ti2 Li3 Li1 59.2(3) . . ?
C2 O1 Ti1 117.5(5) . . ?
C1 O2 Li1 126.2(6) . . ?
C1 O2 Ti1 113.7(5) . . ?
Li1 O2 Ti1 119.5(4) . . ?
C7 O3 Li1 129.0(6) . . ?
C7 O4 C8 116.4(7) . . ?
C9 O5 C10 111.7(7) . . ?
C12 O6 C11 116.1(14) . . ?
C12 O6 Na1 115.0(9) . . ?
C11 O6 Na1 128.8(10) . . ?
C14 O7 C13 112.3(17) . . ?
C14 O7 Na1 111.4(14) . . ?
C13 O7 Na1 107.4(13) . . ?
C16 O8 C15 102.9(16) . . ?
C18 O9 C17 116.2(11) . . ?
C18 O10 Li1 129.3(8) . . ?
C20 O11 Li1 123.6(7) . . ?
C20 O11 Ti2 113.8(5) . . ?
Li1 O11 Ti2 119.4(4) . . ?
C21 O12 Ti2 117.1(6) . . ?
C26 O13 Ti1 116.3(4) . . ?
C25 O14 Li3 122.6(6) . . ?
C25 O14 Ti1 113.7(5) . . ?
Li3 O14 Ti1 119.6(5) . . ?
C31 O15 Li3 129.7(7) . . ?
C31 O16 C32 114.4(6) . . ?
C34 O17 C33 110.3(10) . . ?
C36 O18 C35 125.4(18) . . ?
C37 O19 C38 114.7(18) . . ?
C39 O20 C40 112.0(9) . . ?
C42 O21 C41 119.3(6) . . ?
C42 O22 Li3 128.3(6) . . ?
C44 O23 Li3 122.7(6) . . ?
C44 O23 Ti2 113.0(4) . . ?
Li3 O23 Ti2 121.1(5) . . ?
C45 O24 Ti2 116.3(4) . . ?
C50 O25 Ti1 117.4(5) . . ?
C49 O26 Li2 124.4(7) . . ?
C49 O26 Ti1 113.2(5) . . ?
Li2 O26 Ti1 119.3(4) . . ?
C55 O27 Li2 130.4(8) . . ?
C55 O28 C56 117.6(9) . . ?
C57 O29 C58 103.1(19) . . ?
C57 O29 Na1 109.2(18) . 1_655 ?
C58 O29 Na1 105.1(15) . 1_655 ?
C60 O30 C59 113.8(18) . . ?
C60 O30 Na1 115.8(14) . 1_655 ?
C59 O30 Na1 120.6(13) . 1_655 ?
C61 O31 C62 110.3(14) . . ?
C61 O31 Na1 122.5(11) . 1_655 ?
C62 O31 Na1 127.1(9) . 1_655 ?
C64 O32 C63 112.6(8) . . ?
C66 O33 C65 116.3(7) . . ?
C66 O34 Li2 129.3(6) . . ?
C68 O35 Li2 125.3(6) . . ?
C68 O35 Ti2 113.6(4) . . ?
Li2 O35 Ti2 119.2(5) . . ?
C69 O36 Ti2 118.0(5) . . ?
Na1 O37 H37O 101.6 . . ?
Na1 O37 H37P 148.2 . . ?
H37O O37 H37P 88.8 . . ?
Na1 O38 H38O 99.7 . . ?
Na1 O38 H38P 136.6 . . ?
H38O O38 H38P 105.4 . . ?
O2 C1 C6 126.3(7) . . ?
O2 C1 C2 114.0(7) . . ?
C6 C1 C2 119.7(7) . . ?
O1 C2 C3 123.9(7) . . ?
O1 C2 C1 114.5(7) . . ?
C3 C2 C1 121.5(7) . . ?
C2 C3 C4 118.1(8) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 120.9(8) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.8(8) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 117.8(7) . . ?
C5 C6 C7 121.6(7) . . ?
C1 C6 C7 120.5(7) . . ?
O3 C7 O4 122.3(7) . . ?
O3 C7 C6 126.0(7) . . ?
O4 C7 C6 111.7(7) . . ?
O4 C8 C9 107.3(7) . . ?
O4 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
O4 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
O5 C9 C8 109.3(8) . . ?
O5 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
O5 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
O5 C10 C11 110.2(10) . . ?
O5 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
O5 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O6 C11 C10 111.8(12) . . ?
O6 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
O6 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
O6 C12 C13 115.9(17) . . ?
O6 C12 H12A 108.3 . . ?
C13 C12 H12A 108.3 . . ?
O6 C12 H12B 108.3 . . ?
C13 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
O7 C13 C12 111.7(18) . . ?
O7 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
O7 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
O7 C14 C15 106.8(18) . . ?
O7 C14 H14A 110.4 . . ?
C15 C14 H14A 110.4 . . ?
O7 C14 H14B 110.4 . . ?
C15 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
O8 C15 C14 102.3(17) . . ?
O8 C15 Na1 151.9(19) . . ?
C14 C15 Na1 84.4(13) . . ?
O8 C15 H15A 111.3 . . ?
C14 C15 H15A 111.3 . . ?
Na1 C15 H15A 90.7 . . ?
O8 C15 H15B 111.3 . . ?
C14 C15 H15B 111.3 . . ?
Na1 C15 H15B 42.4 . . ?
H15A C15 H15B 109.2 . . ?
O8 C16 C17 132(2) . . ?
O8 C16 H16A 104.3 . . ?
C17 C16 H16A 104.3 . . ?
O8 C16 H16B 104.3 . . ?
C17 C16 H16B 104.3 . . ?
H16A C16 H16B 105.6 . . ?
O9 C17 C16 107.4(15) . . ?
O9 C17 H17A 110.2 . . ?
C16 C17 H17A 110.2 . . ?
O9 C17 H17B 110.2 . . ?
C16 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?
O10 C18 O9 122.5(10) . . ?
O10 C18 C19 125.4(8) . . ?
O9 C18 C19 112.1(9) . . ?
C20 C19 C24 118.2(10) . . ?
C20 C19 C18 121.2(8) . . ?
C24 C19 C18 120.5(9) . . ?
O11 C20 C19 126.8(9) . . ?
O11 C20 C21 113.1(8) . . ?
C19 C20 C21 120.0(8) . . ?
O12 C21 C22 123.8(10) . . ?
O12 C21 C20 115.1(7) . . ?
C22 C21 C20 121.1(10) . . ?
C21 C22 C23 118.5(11) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 121.8(9) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C19 120.4(10) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
O14 C25 C30 127.3(7) . . ?
O14 C25 C26 112.6(7) . . ?
C30 C25 C26 120.0(7) . . ?
O13 C26 C27 123.6(7) . . ?
O13 C26 C25 115.8(7) . . ?
C27 C26 C25 120.7(7) . . ?
C26 C27 C28 119.4(7) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 119.7(7) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 121.3(8) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C25 C30 C29 118.9(7) . . ?
C25 C30 C31 120.6(6) . . ?
C29 C30 C31 120.5(7) . . ?
O15 C31 O16 121.6(7) . . ?
O15 C31 C30 125.6(7) . . ?
O16 C31 C30 112.8(6) . . ?
O16 C32 C33 107.3(6) . . ?
O16 C32 H32A 110.3 . . ?
C33 C32 H32A 110.3 . . ?
O16 C32 H32B 110.3 . . ?
C33 C32 H32B 110.3 . . ?
H32A C32 H32B 108.5 . . ?
O17 C33 C32 107.5(8) . . ?
O17 C33 H33A 110.2 . . ?
C32 C33 H33A 110.2 . . ?
O17 C33 H33B 110.2 . . ?
C32 C33 H33B 110.2 . . ?
H33A C33 H33B 108.5 . . ?
C35 C34 O17 106.6(14) . . ?
C35 C34 H34A 110.4 . . ?
O17 C34 H34A 110.4 . . ?
C35 C34 H34B 110.4 . . ?
O17 C34 H34B 110.4 . . ?
H34A C34 H34B 108.6 . . ?
O18 C35 C34 121.2(17) . . ?
O18 C35 H35A 107.0 . . ?
C34 C35 H35A 107.0 . . ?
O18 C35 H35B 107.0 . . ?
C34 C35 H35B 107.0 . . ?
H35A C35 H35B 106.8 . . ?
O18 C36 C37 114.8(19) . . ?
O18 C36 H36A 108.6 . . ?
C37 C36 H36A 108.6 . . ?
O18 C36 H36B 108.6 . . ?
C37 C36 H36B 108.6 . . ?
H36A C36 H36B 107.5 . . ?
C36 C37 O19 114.8(18) . . ?
C36 C37 H37A 108.6 . . ?
O19 C37 H37A 108.6 . . ?
C36 C37 H37B 108.6 . . ?
O19 C37 H37B 108.6 . . ?
H37A C37 H37B 107.5 . . ?
C39 C38 O19 111.2(17) . . ?
C39 C38 H38A 109.4 . . ?
O19 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
O19 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C38 C39 O20 107.7(13) . . ?
C38 C39 H39A 110.2 . . ?
O20 C39 H39A 110.2 . . ?
C38 C39 H39B 110.2 . . ?
O20 C39 H39B 110.2 . . ?
H39A C39 H39B 108.5 . . ?
C41 C40 O20 107.9(9) . . ?
C41 C40 H40A 110.1 . . ?
O20 C40 H40A 110.1 . . ?
C41 C40 H40B 110.1 . . ?
O20 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
O21 C41 C40 109.2(7) . . ?
O21 C41 H41A 109.8 . . ?
C40 C41 H41A 109.8 . . ?
O21 C41 H41B 109.8 . . ?
C40 C41 H41B 109.8 . . ?
H41A C41 H41B 108.3 . . ?
O22 C42 O21 122.3(7) . . ?
O22 C42 C43 124.8(7) . . ?
O21 C42 C43 112.9(6) . . ?
C44 C43 C48 118.7(6) . . ?
C44 C43 C42 122.9(6) . . ?
C48 C43 C42 118.4(7) . . ?
O23 C44 C43 126.4(6) . . ?
O23 C44 C45 113.5(6) . . ?
C43 C44 C45 120.1(6) . . ?
O24 C45 C46 123.2(7) . . ?
O24 C45 C44 115.4(6) . . ?
C46 C45 C44 121.4(7) . . ?
C45 C46 C47 118.3(7) . . ?
C45 C46 H46 120.8 . . ?
C47 C46 H46 120.8 . . ?
C48 C47 C46 121.3(7) . . ?
C48 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
C47 C48 C43 120.3(7) . . ?
C47 C48 H48 119.9 . . ?
C43 C48 H48 119.9 . . ?
O26 C49 C50 114.4(8) . . ?
O26 C49 C54 125.7(8) . . ?
C50 C49 C54 119.8(8) . . ?
O25 C50 C51 124.8(9) . . ?
O25 C50 C49 115.0(7) . . ?
C51 C50 C49 120.2(9) . . ?
C52 C51 C50 119.4(11) . . ?
C52 C51 H51 120.3 . . ?
C50 C51 H51 120.3 . . ?
C51 C52 C53 122.2(10) . . ?
C51 C52 H52 118.9 . . ?
C53 C52 H52 118.9 . . ?
C52 C53 C54 120.0(11) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C53 C54 C49 118.2(10) . . ?
C53 C54 C55 121.5(9) . . ?
C49 C54 C55 120.3(8) . . ?
O27 C55 O28 123.1(9) . . ?
O27 C55 C54 125.6(8) . . ?
O28 C55 C54 111.2(8) . . ?
O28 C56 C57 110.9(17) . . ?
O28 C56 H56A 109.5 . . ?
C57 C56 H56A 109.5 . . ?
O28 C56 H56B 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56A C56 H56B 108.0 . . ?
O29 C57 C56 113(2) . . ?
O29 C57 H57A 108.9 . . ?
C56 C57 H57A 108.9 . . ?
O29 C57 H57B 108.9 . . ?
C56 C57 H57B 108.9 . . ?
H57A C57 H57B 107.7 . . ?
C59 C58 O29 104(2) . . ?
C59 C58 H58A 111.0 . . ?
O29 C58 H58A 111.0 . . ?
C59 C58 H58B 111.0 . . ?
O29 C58 H58B 111.0 . . ?
H58A C58 H58B 109.0 . . ?
C58 C59 O30 109.7(19) . . ?
C58 C59 H59A 109.7 . . ?
O30 C59 H59A 109.7 . . ?
C58 C59 H59B 109.7 . . ?
O30 C59 H59B 109.7 . . ?
H59A C59 H59B 108.2 . . ?
O30 C60 C61 116(2) . . ?
O30 C60 H60A 108.3 . . ?
C61 C60 H60A 108.3 . . ?
O30 C60 H60B 108.3 . . ?
C61 C60 H60B 108.3 . . ?
H60A C60 H60B 107.4 . . ?
O31 C61 C60 107.8(19) . . ?
O31 C61 H61A 110.2 . . ?
C60 C61 H61A 110.2 . . ?
O31 C61 H61B 110.2 . . ?
C60 C61 H61B 110.2 . . ?
H61A C61 H61B 108.5 . . ?
O31 C62 C63 112.3(12) . . ?
O31 C62 H62A 109.1 . . ?
C63 C62 H62A 109.1 . . ?
O31 C62 H62B 109.1 . . ?
C63 C62 H62B 109.1 . . ?
H62A C62 H62B 107.9 . . ?
O32 C63 C62 110.2(14) . . ?
O32 C63 H63A 109.6 . . ?
C62 C63 H63A 109.6 . . ?
O32 C63 H63B 109.6 . . ?
C62 C63 H63B 109.6 . . ?
H63A C63 H63B 108.1 . . ?
O32 C64 C65 108.0(8) . . ?
O32 C64 H64A 110.1 . . ?
C65 C64 H64A 110.1 . . ?
O32 C64 H64B 110.1 . . ?
C65 C64 H64B 110.1 . . ?
H64A C64 H64B 108.4 . . ?
O33 C65 C64 107.6(8) . . ?
O33 C65 H65A 110.2 . . ?
C64 C65 H65A 110.2 . . ?
O33 C65 H65B 110.2 . . ?
C64 C65 H65B 110.2 . . ?
H65A C65 H65B 108.5 . . ?
O34 C66 O33 121.7(7) . . ?
O34 C66 C67 125.6(7) . . ?
O33 C66 C67 112.6(7) . . ?
C72 C67 C68 118.4(7) . . ?
C72 C67 C66 120.3(7) . . ?
C68 C67 C66 121.3(7) . . ?
O35 C68 C69 114.9(6) . . ?
O35 C68 C67 125.8(7) . . ?
C69 C68 C67 119.3(7) . . ?
O36 C69 C70 124.7(7) . . ?
O36 C69 C68 113.3(7) . . ?
C70 C69 C68 122.0(7) . . ?
C71 C70 C69 118.6(8) . . ?
C71 C70 H70 120.7 . . ?
C69 C70 H70 120.7 . . ?
C70 C71 C72 121.2(8) . . ?
C70 C71 H71 119.4 . . ?
C72 C71 H71 119.4 . . ?
C67 C72 C71 120.4(8) . . ?
C67 C72 H72 119.8 . . ?
C71 C72 H72 119.8 . . ?
C73 N1 C74 122(2) . . ?
C73 N1 C75 120.3(18) . . ?
C74 N1 C75 117.7(18) . . ?
O39 C73 N1 131(2) . . ?
O39 C73 H73 114.5 . . ?
N1 C73 H73 114.5 . . ?
N1 C74 H74A 109.5 . . ?
N1 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
N1 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N1 C75 H75A 109.5 . . ?
N1 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N1 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
H40O O40 H40P 125.0 . . ?
C77 N2 C76 122.8(14) . . ?
C77 N2 C78 117.3(14) . . ?
C76 N2 C78 119.8(13) . . ?
O41 C76 N2 119.8(19) . . ?
O41 C76 H76 120.1 . . ?
N2 C76 H76 120.1 . . ?
N2 C77 H77A 109.5 . . ?
N2 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
N2 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N2 C78 H78A 109.5 . . ?
N2 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
N2 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.897(6) . ?
Ti1 O25 1.908(6) . ?
Ti1 O13 1.914(5) . ?
Ti1 O14 2.021(5) . ?
Ti1 O2 2.022(5) . ?
Ti1 O26 2.034(5) . ?
Ti1 Li1 3.409(12) . ?
Ti1 Li2 3.436(14) . ?
Ti1 Li3 3.452(13) . ?
Ti2 O36 1.893(6) . ?
Ti2 O12 1.901(6) . ?
Ti2 O24 1.907(5) . ?
Ti2 O35 2.012(5) . ?
Ti2 O11 2.023(6) . ?
Ti2 O23 2.032(5) . ?
Ti2 Li2 3.412(13) . ?
Ti2 Li1 3.430(13) . ?
Ti2 Li3 3.459(13) . ?
Na1 O38 2.375(16) . ?
Na1 O37 2.38(2) . ?
Na1 O6 2.516(16) . ?
Na1 O7 2.566(13) . ?
Na1 O30 2.614(18) 1_455 ?
Na1 O31 2.625(16) 1_455 ?
Na1 O29 2.80(2) 1_455 ?
Na1 C15 3.12(2) . ?
Na1 H38O 2.6499 . ?
Li1 O2 1.925(13) . ?
Li1 O10 1.934(13) . ?
Li1 O11 1.950(13) . ?
Li1 O3 1.965(13) . ?
Li1 Li3 3.485(17) . ?
Li2 O27 1.912(14) . ?
Li2 O35 1.944(14) . ?
Li2 O26 1.947(15) . ?
Li2 O34 1.948(15) . ?
Li3 O15 1.928(15) . ?
Li3 O22 1.929(15) . ?
Li3 O23 1.940(14) . ?
Li3 O14 1.973(14) . ?
O1 C2 1.350(10) . ?
O2 C1 1.344(9) . ?
O3 C7 1.221(10) . ?
O4 C7 1.338(10) . ?
O4 C8 1.451(10) . ?
O5 C9 1.410(13) . ?
O5 C10 1.429(11) . ?
O6 C12 1.321(18) . ?
O6 C11 1.393(17) . ?
O7 C14 1.39(2) . ?
O7 C13 1.42(3) . ?
O8 C16 1.32(2) . ?
O8 C15 1.428(18) . ?
O9 C18 1.349(11) . ?
O9 C17 1.35(2) . ?
O10 C18 1.212(12) . ?
O11 C20 1.337(9) . ?
O12 C21 1.333(12) . ?
O13 C26 1.330(10) . ?
O14 C25 1.347(9) . ?
O15 C31 1.214(9) . ?
O16 C31 1.335(9) . ?
O16 C32 1.451(9) . ?
O17 C34 1.410(17) . ?
O17 C33 1.417(13) . ?
O18 C36 1.27(2) . ?
O18 C35 1.36(2) . ?
O19 C37 1.44(2) . ?
O19 C38 1.47(2) . ?
O20 C39 1.470(16) . ?
O20 C40 1.471(14) . ?
O21 C42 1.332(10) . ?
O21 C41 1.449(9) . ?
O22 C42 1.214(9) . ?
O23 C44 1.358(8) . ?
O24 C45 1.358(9) . ?
O25 C50 1.330(10) . ?
O26 C49 1.333(10) . ?
O27 C55 1.194(11) . ?
O28 C55 1.342(11) . ?
O28 C56 1.434(17) . ?
O29 C57 1.33(3) . ?
O29 C58 1.432(19) . ?
O30 C60 1.32(3) . ?
O30 C59 1.487(19) . ?
O31 C61 1.397(19) . ?
O31 C62 1.462(18) . ?
O32 C64 1.377(11) . ?
O32 C63 1.408(18) . ?
O33 C66 1.329(10) . ?
O33 C65 1.465(11) . ?
O34 C66 1.213(10) . ?
O35 C68 1.333(9) . ?
O36 C69 1.350(9) . ?
O37 H37O 0.8400 . ?
O37 H37P 0.8400 . ?
O38 H38O 0.8400 . ?
O38 H38P 0.8401 . ?
C1 C6 1.406(11) . ?
C1 C2 1.416(11) . ?
C2 C3 1.379(12) . ?
C3 C4 1.407(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.403(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.474(11) . ?
C8 C9 1.501(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.489(18) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.47(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.51(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.425(18) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.470(15) . ?
C19 C20 1.384(13) . ?
C19 C24 1.430(14) . ?
C20 C21 1.431(14) . ?
C21 C22 1.375(12) . ?
C22 C23 1.396(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(18) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.390(11) . ?
C25 C26 1.429(11) . ?
C26 C27 1.379(11) . ?
C27 C28 1.417(13) . ?
C27 H27 0.9500 . ?
C28 C29 1.393(12) . ?
C28 H28 0.9500 . ?
C29 C30 1.407(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.476(10) . ?
C32 C33 1.485(12) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.428(19) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.377(19) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.47(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.460(14) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.484(10) . ?
C43 C44 1.366(11) . ?
C43 C48 1.423(10) . ?
C44 C45 1.410(10) . ?
C45 C46 1.379(11) . ?
C46 C47 1.388(12) . ?
C46 H46 0.9500 . ?
C47 C48 1.374(11) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.405(13) . ?
C49 C54 1.415(12) . ?
C50 C51 1.380(12) . ?
C51 C52 1.369(17) . ?
C51 H51 0.9500 . ?
C52 C53 1.369(18) . ?
C52 H52 0.9500 . ?
C53 C54 1.408(14) . ?
C53 H53 0.9500 . ?
C54 C55 1.473(14) . ?
C56 C57 1.50(2) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.41(2) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.51(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.505(17) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.509(13) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.473(12) . ?
C67 C72 1.404(12) . ?
C67 C68 1.410(11) . ?
C68 C69 1.407(11) . ?
C69 C70 1.383(12) . ?
C70 C71 1.378(12) . ?
C70 H70 0.9500 . ?
C71 C72 1.406(13) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
O39 C73 1.27(2) . ?
N1 C73 1.31(3) . ?
N1 C74 1.43(2) . ?
N1 C75 1.46(2) . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
O40 H40O 0.8399 . ?
O40 H40P 0.8397 . ?
O41 C76 1.243(18) . ?
N2 C77 1.38(2) . ?
N2 C76 1.38(2) . ?
N2 C78 1.420(16) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
