#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:00:16 +0200 (lun 05 de abr de 2021) $
#$Revision: 263793 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/67/7706777.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_7706777
loop_
_publ_author_name
'Xing, Tian'
'Prior, Timothy J.'
'Chen, Kai'
'Redshaw, Carl'
_publ_section_title
;
 Titanium complexes bearing oxa- and azacalix[4, 6]arenes: structural
 studies and use in the ring opening homo-/co-polymerization of cyclic
 esters.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4396
_journal_page_last               4407
_journal_paper_doi               10.1039/d1dt00189b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
;
 C52 H60 Br4 N2 O9 Ti2, 2(C2 H3 N) [+ 2.5MeCN] 
;
_chemical_formula_sum            'C56 H66 Br4 N4 O9 Ti2'
_chemical_formula_weight         1354.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                111.546(5)
_cell_angle_beta                 94.299(6)
_cell_angle_gamma                96.876(5)
_cell_formula_units_Z            2
_cell_length_a                   12.8059(9)
_cell_length_b                   14.7294(9)
_cell_length_c                   18.6847(13)
_cell_measurement_reflns_used    18942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      1.50
_cell_volume                     3227.4(4)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25790
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'fine-fosu sealed tube'
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Face index absorption correction within 
Stoe X-AREA (Tompa method)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;

Solvent is MeCN (22 electrons) 110 electrons in the cell
equates to 5 MeCN and hence 2.5 per asym unit. 
;
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         13079
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0458
_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)+(0.0511P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8355
_reflns_number_total             13079
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00189b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7706773--7706779.cif.'
_cod_database_code               7706777
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2016/6
_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   0.435
_shelx_estimated_absorpt_t_max   0.607
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.6836(3) 0.7545(3) 0.2064(2) 0.0256(9) Uani 1 1 d . . . . .
C2 C 0.6161(3) 0.8100(3) 0.2544(2) 0.0263(9) Uani 1 1 d . . . . .
C3 C 0.5607(4) 0.8706(3) 0.2286(3) 0.0323(10) Uani 1 1 d . . . . .
H3 H 0.515725 0.909074 0.261230 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5693(4) 0.8765(3) 0.1571(3) 0.0373(12) Uani 1 1 d . . . . .
C5 C 0.6349(4) 0.8179(3) 0.1096(3) 0.0354(11) Uani 1 1 d . . . . .
H5 H 0.642008 0.821257 0.060333 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6899(4) 0.7552(3) 0.1321(2) 0.0294(10) Uani 1 1 d . . . . .
C7 C 0.5121(5) 0.9455(4) 0.1314(3) 0.0539(16) Uani 1 1 d . . . . .
H7A H 0.559685 1.007937 0.143727 0.081 Uiso 1 1 calc R U . . .
H7B H 0.449472 0.958268 0.158425 0.081 Uiso 1 1 calc R U . . .
H7C H 0.489881 0.914905 0.075260 0.081 Uiso 1 1 calc R U . . .
C8 C 0.7549(3) 0.6893(3) 0.0770(2) 0.0294(10) Uani 1 1 d . . . . .
H8A H 0.813478 0.676353 0.107776 0.035 Uiso 1 1 calc R U . . .
H8B H 0.786955 0.725018 0.046305 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6666(3) 0.5122(3) 0.0452(2) 0.0293(10) Uani 1 1 d . . . . .
C11 C 0.6926(3) 0.5910(3) 0.0216(3) 0.0299(10) Uani 1 1 d . . . . .
C12 C 0.6584(4) 0.5752(3) -0.0549(2) 0.0327(10) Uani 1 1 d . . . . .
H12 H 0.673192 0.628038 -0.072098 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6031(4) 0.4850(4) -0.1077(3) 0.0380(12) Uani 1 1 d . . . . .
C14 C 0.5822(4) 0.4077(4) -0.0829(3) 0.0343(11) Uani 1 1 d . . . . .
H14 H 0.546281 0.345113 -0.118176 0.041 Uiso 1 1 calc R U . . .
C15 C 0.6138(3) 0.4219(3) -0.0062(2) 0.0279(10) Uani 1 1 d . . . . .
C17 C 0.5670(6) 0.4705(4) -0.1913(3) 0.0612(18) Uani 1 1 d . . . . .
H17A H 0.490555 0.471223 -0.197984 0.092 Uiso 1 1 calc R U . . .
H17B H 0.582578 0.406872 -0.226440 0.092 Uiso 1 1 calc R U . . .
H17C H 0.604800 0.524014 -0.203301 0.092 Uiso 1 1 calc R U . . .
C18 C 0.5891(3) 0.3387(3) 0.0220(3) 0.0298(10) Uani 1 1 d . . . . .
H18A H 0.551342 0.279322 -0.021643 0.036 Uiso 1 1 calc R U . . .
H18B H 0.541506 0.358064 0.062617 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7637(4) 0.2863(4) -0.0035(3) 0.0403(12) Uani 1 1 d . . . . .
H19A H 0.729818 0.228485 -0.048943 0.060 Uiso 1 1 calc R U . . .
H19B H 0.827156 0.270635 0.019329 0.060 Uiso 1 1 calc R U . . .
H19C H 0.783991 0.341827 -0.019302 0.060 Uiso 1 1 calc R U . . .
C20 C 0.6664(3) 0.2330(3) 0.0860(2) 0.0270(9) Uani 1 1 d . . . . .
H20A H 0.650670 0.168344 0.041884 0.032 Uiso 1 1 calc R U . . .
H20B H 0.731295 0.232785 0.118284 0.032 Uiso 1 1 calc R U . . .
C21 C 0.5834(3) 0.3254(3) 0.2032(2) 0.0216(9) Uani 1 1 d . . . . .
C22 C 0.5765(3) 0.2435(3) 0.1335(2) 0.0244(9) Uani 1 1 d . . . . .
C23 C 0.4878(3) 0.1710(3) 0.1106(2) 0.0281(10) Uani 1 1 d . . . . .
H23 H 0.483170 0.115956 0.063006 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4047(3) 0.1769(3) 0.1558(3) 0.0281(10) Uani 1 1 d . . . . .
C25 C 0.4138(3) 0.2605(3) 0.2237(2) 0.0257(9) Uani 1 1 d . . . . .
H25 H 0.357853 0.265919 0.254953 0.031 Uiso 1 1 calc R U . . .
C26 C 0.4997(3) 0.3363(3) 0.2486(2) 0.0240(9) Uani 1 1 d . . . . .
C27 C 0.3093(3) 0.0968(4) 0.1314(3) 0.0390(12) Uani 1 1 d . . . . .
H27A H 0.293214 0.079649 0.175754 0.058 Uiso 1 1 calc R U . . .
H27B H 0.324382 0.038259 0.089505 0.058 Uiso 1 1 calc R U . . .
H27C H 0.248371 0.120427 0.113064 0.058 Uiso 1 1 calc R U . . .
C28 C 0.5035(3) 0.4262(3) 0.3214(2) 0.0238(9) Uani 1 1 d . . . . .
H28A H 0.431089 0.442839 0.326893 0.029 Uiso 1 1 calc R U . . .
H28B H 0.548726 0.482749 0.316916 0.029 Uiso 1 1 calc R U . . .
C29 C 0.6551(3) 0.4380(3) 0.4220(2) 0.0221(9) Uani 1 1 d . . . . .
C30 C 0.5465(3) 0.4113(3) 0.3935(2) 0.0214(8) Uani 1 1 d . . . . .
C31 C 0.4796(3) 0.3721(3) 0.4330(2) 0.0255(9) Uani 1 1 d . . . . .
H31 H 0.406045 0.354264 0.414338 0.031 Uiso 1 1 calc R U . . .
C32 C 0.5168(3) 0.3578(3) 0.4995(2) 0.0256(9) Uani 1 1 d . . . . .
C33 C 0.6234(3) 0.3867(3) 0.5266(2) 0.0265(9) Uani 1 1 d . . . . .
H33 H 0.649452 0.377971 0.572237 0.032 Uiso 1 1 calc R U . . .
C34 C 0.6944(3) 0.4279(3) 0.4902(2) 0.0255(9) Uani 1 1 d . . . . .
C35 C 0.4421(3) 0.3125(4) 0.5400(3) 0.0341(11) Uani 1 1 d . . . . .
H35A H 0.370241 0.297008 0.512134 0.051 Uiso 1 1 calc R U . . .
H35B H 0.464791 0.251613 0.540856 0.051 Uiso 1 1 calc R U . . .
H35C H 0.442564 0.359199 0.593260 0.051 Uiso 1 1 calc R U . . .
C36 C 0.8093(3) 0.4624(3) 0.5250(2) 0.0242(9) Uani 1 1 d . . . . .
H36A H 0.853439 0.462632 0.483733 0.029 Uiso 1 1 calc R U . . .
H36B H 0.832997 0.415864 0.547465 0.029 Uiso 1 1 calc R U . . .
C37 C 0.8324(3) 0.6505(3) 0.5697(2) 0.0235(9) Uani 1 1 d . . . . .
C38 C 0.8246(3) 0.5658(3) 0.5879(2) 0.0254(9) Uani 1 1 d . . . . .
C39 C 0.8305(3) 0.5808(3) 0.6661(2) 0.0277(10) Uani 1 1 d . . . . .
H39 H 0.824359 0.524422 0.679753 0.033 Uiso 1 1 calc R U . . .
C40 C 0.8448(3) 0.6733(4) 0.7251(2) 0.0295(10) Uani 1 1 d . . . . .
C41 C 0.8557(3) 0.7555(4) 0.7041(3) 0.0311(10) Uani 1 1 d . . . . .
H41 H 0.868599 0.820028 0.743517 0.037 Uiso 1 1 calc R U . . .
C42 C 0.8481(3) 0.7446(3) 0.6270(3) 0.0277(10) Uani 1 1 d . . . . .
C43 C 0.8466(4) 0.6864(4) 0.8097(3) 0.0392(12) Uani 1 1 d . . . . .
H43A H 0.777094 0.699104 0.826110 0.059 Uiso 1 1 calc R U . . .
H43B H 0.900974 0.742466 0.841627 0.059 Uiso 1 1 calc R U . . .
H43C H 0.862933 0.626207 0.815863 0.059 Uiso 1 1 calc R U . . .
C44 C 0.8542(3) 0.8335(3) 0.6049(3) 0.0302(10) Uani 1 1 d . . . . .
H44A H 0.783471 0.835351 0.580589 0.036 Uiso 1 1 calc R U . . .
H44B H 0.873890 0.894342 0.652321 0.036 Uiso 1 1 calc R U . . .
C45 C 1.0429(3) 0.8333(4) 0.5844(3) 0.0349(11) Uani 1 1 d . . . . .
H45A H 1.065734 0.895853 0.628786 0.052 Uiso 1 1 calc R U . . .
H45B H 1.091903 0.826826 0.545595 0.052 Uiso 1 1 calc R U . . .
H45C H 1.042682 0.778136 0.601846 0.052 Uiso 1 1 calc R U . . .
C46 C 0.9358(3) 0.9170(3) 0.5221(3) 0.0265(9) Uani 1 1 d . . . . .
H46A H 0.970592 0.978241 0.565390 0.032 Uiso 1 1 calc R U . . .
H46B H 0.980146 0.905055 0.479380 0.032 Uiso 1 1 calc R U . . .
C47 C 0.7691(3) 0.8628(3) 0.4282(2) 0.0225(9) Uani 1 1 d . . . . .
C48 C 0.8297(3) 0.9337(3) 0.4945(2) 0.0232(9) Uani 1 1 d . . . . .
C49 C 0.7947(3) 1.0224(3) 0.5319(2) 0.0277(9) Uani 1 1 d . . . . .
H49 H 0.837017 1.070967 0.576544 0.033 Uiso 1 1 calc R U . . .
C50 C 0.6981(3) 1.0419(3) 0.5052(3) 0.0301(10) Uani 1 1 d . . . . .
C51 C 0.6380(3) 0.9683(3) 0.4405(2) 0.0271(9) Uani 1 1 d . . . . .
H51 H 0.571265 0.979863 0.422778 0.033 Uiso 1 1 calc R U . . .
C52 C 0.6702(3) 0.8792(3) 0.4006(2) 0.0226(9) Uani 1 1 d . . . . .
C53 C 0.6622(4) 1.1408(4) 0.5474(3) 0.0452(13) Uani 1 1 d . . . . .
H53A H 0.715816 1.181830 0.591270 0.068 Uiso 1 1 calc R U . . .
H53B H 0.653023 1.174670 0.511553 0.068 Uiso 1 1 calc R U . . .
H53C H 0.594636 1.129423 0.566610 0.068 Uiso 1 1 calc R U . . .
C54 C 0.6011(3) 0.8011(3) 0.3309(2) 0.0266(9) Uani 1 1 d . . . . .
H54A H 0.615554 0.735330 0.327820 0.032 Uiso 1 1 calc R U . . .
H54B H 0.525888 0.804213 0.339166 0.032 Uiso 1 1 calc R U . . .
C61 C 0.8036(6) 0.0291(4) 0.1263(4) 0.0656(19) Uani 1 1 d . . . . .
C62 C 0.8350(6) 0.0243(4) 0.2003(3) 0.0632(18) Uani 1 1 d . . . . .
H62A H 0.865853 -0.035906 0.192300 0.095 Uiso 1 1 calc R U . . .
H62B H 0.772778 0.023257 0.227701 0.095 Uiso 1 1 calc R U . . .
H62C H 0.887686 0.082284 0.231341 0.095 Uiso 1 1 calc R U . . .
C63 C 0.5805(4) 0.1524(4) 0.3375(3) 0.0461(13) Uani 1 1 d . . . . .
H63A H 0.623919 0.100280 0.331819 0.069 Uiso 1 1 calc R U . . .
H63B H 0.607705 0.209476 0.385421 0.069 Uiso 1 1 calc R U . . .
H63C H 0.583444 0.172345 0.293032 0.069 Uiso 1 1 calc R U . . .
C64 C 0.4722(4) 0.1156(4) 0.3408(3) 0.0450(12) Uani 1 1 d . . . . .
N1 N 0.6884(3) 0.3137(3) 0.0547(2) 0.0271(8) Uani 1 1 d . . . . .
H1 H 0.724170 0.374683 0.098967 0.032 Uiso 1 1 calc R U . . .
N2 N 0.9341(3) 0.8318(3) 0.5494(2) 0.0259(8) Uani 1 1 d . . . . .
H2 H 0.914068 0.768883 0.502812 0.031 Uiso 1 1 calc R U . . .
N3 N 0.7785(7) 0.0327(5) 0.0686(3) 0.113(3) Uani 1 1 d . . . . .
N4 N 0.3861(4) 0.0881(4) 0.3427(4) 0.0741(16) Uani 1 1 d . . . . .
O1 O 0.7383(2) 0.6950(2) 0.22990(16) 0.0276(7) Uani 1 1 d . . . . .
O2 O 0.6951(3) 0.5158(2) 0.11815(16) 0.0330(7) Uani 1 1 d . . . . .
H2A H 0.722685 0.573787 0.147047 0.050 Uiso 1 1 calc R U . . .
O3 O 0.6701(2) 0.3967(2) 0.22417(15) 0.0227(6) Uani 1 1 d . . . . .
O4 O 0.7229(2) 0.4796(2) 0.38555(15) 0.0242(6) Uani 1 1 d . . . . .
O5 O 0.8264(2) 0.6464(2) 0.49521(16) 0.0297(7) Uani 1 1 d . . . . .
H5A H 0.803274 0.588185 0.464334 0.045 Uiso 1 1 calc R U . . .
O6 O 0.8037(2) 0.7756(2) 0.39160(15) 0.0234(6) Uani 1 1 d . . . . .
O7 O 0.8116(2) 0.5778(2) 0.29986(15) 0.0218(6) Uani 1 1 d . . . . .
Br1 Br 1.03835(3) 0.70528(3) 0.37956(3) 0.03043(11) Uani 1 1 d . . . . .
Br2 Br 0.93998(4) 0.86380(4) 0.29109(3) 0.03535(12) Uani 1 1 d . . . . .
Br3 Br 0.81039(4) 0.28108(3) 0.29815(3) 0.03491(12) Uani 1 1 d . . . . .
Br4 Br 0.90993(3) 0.40720(4) 0.18148(3) 0.03278(12) Uani 1 1 d . . . . .
Ti1 Ti 0.85229(6) 0.70154(6) 0.30237(4) 0.02240(16) Uani 1 1 d . . . . .
Ti2 Ti 0.78827(5) 0.45158(6) 0.29535(4) 0.02106(16) Uani 1 1 d . . . . .
O9 O 0.9373(2) 0.4911(2) 0.36903(18) 0.0281(7) Uani 1 1 d D . . . .
O8 O 0.9298(2) 0.6332(2) 0.20359(18) 0.0322(7) Uani 1 1 d D . . . .
H8C H 0.932(4) 0.574(2) 0.196(3) 0.048 Uiso 1 1 d D U . . .
H8D H 0.993(3) 0.654(3) 0.203(3) 0.048 Uiso 1 1 d D U . . .
H9A H 0.966(4) 0.549(2) 0.382(3) 0.048 Uiso 1 1 d D U . . .
H9B H 0.977(3) 0.452(3) 0.353(3) 0.048 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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 C1 C6 119.4(4) . . ?
O1 C1 C2 120.0(4) . . ?
C6 C1 C2 120.4(4) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C54 121.0(4) . . ?
C1 C2 C54 120.3(4) . . ?
C4 C3 C2 122.2(5) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 117.8(4) . . ?
C3 C4 C7 121.4(5) . . ?
C5 C4 C7 120.8(4) . . ?
C6 C5 C4 122.2(4) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 118.6(4) . . ?
C5 C6 C8 120.2(4) . . ?
C1 C6 C8 121.2(4) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 C11 114.4(4) . . ?
C6 C8 H8A 108.7 . . ?
C11 C8 H8A 108.7 . . ?
C6 C8 H8B 108.7 . . ?
C11 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O2 C10 C15 114.6(4) . . ?
O2 C10 C11 123.9(4) . . ?
C15 C10 C11 121.4(4) . . ?
C12 C11 C10 116.8(4) . . ?
C12 C11 C8 121.5(4) . . ?
C10 C11 C8 121.6(4) . . ?
C11 C12 C13 122.8(4) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 118.6(4) . . ?
C14 C13 C17 120.1(4) . . ?
C12 C13 C17 121.2(4) . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C10 C15 C14 120.4(4) . . ?
C10 C15 C18 119.3(4) . . ?
C14 C15 C18 120.3(4) . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 N1 111.9(3) . . ?
C15 C18 H18A 109.2 . . ?
N1 C18 H18A 109.2 . . ?
C15 C18 H18B 109.2 . . ?
N1 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 N1 114.1(3) . . ?
C22 C20 H20A 108.7 . . ?
N1 C20 H20A 108.7 . . ?
C22 C20 H20B 108.7 . . ?
N1 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
O3 C21 C22 118.8(4) . . ?
O3 C21 C26 120.4(4) . . ?
C22 C21 C26 120.7(4) . . ?
C23 C22 C21 119.5(4) . . ?
C23 C22 C20 120.5(4) . . ?
C21 C22 C20 119.9(4) . . ?
C22 C23 C24 121.5(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C25 C24 C23 117.0(4) . . ?
C25 C24 C27 121.7(4) . . ?
C23 C24 C27 121.3(4) . . ?
C26 C25 C24 123.9(4) . . ?
C26 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
C25 C26 C21 117.3(4) . . ?
C25 C26 C28 121.4(4) . . ?
C21 C26 C28 121.3(4) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 C30 112.6(3) . . ?
C26 C28 H28A 109.1 . . ?
C30 C28 H28A 109.1 . . ?
C26 C28 H28B 109.1 . . ?
C30 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
O4 C29 C34 119.0(3) . . ?
O4 C29 C30 119.9(3) . . ?
C34 C29 C30 121.0(4) . . ?
C31 C30 C29 118.5(4) . . ?
C31 C30 C28 120.7(3) . . ?
C29 C30 C28 120.9(4) . . ?
C30 C31 C32 121.9(4) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 117.9(4) . . ?
C33 C32 C35 121.6(4) . . ?
C31 C32 C35 120.5(4) . . ?
C32 C33 C34 122.9(4) . . ?
C32 C33 H33 118.5 . . ?
C34 C33 H33 118.5 . . ?
C33 C34 C29 117.7(4) . . ?
C33 C34 C36 120.2(4) . . ?
C29 C34 C36 122.1(4) . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 C38 111.0(3) . . ?
C34 C36 H36A 109.4 . . ?
C38 C36 H36A 109.4 . . ?
C34 C36 H36B 109.4 . . ?
C38 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
O5 C37 C42 115.5(4) . . ?
O5 C37 C38 122.9(4) . . ?
C42 C37 C38 121.6(4) . . ?
C39 C38 C37 116.8(4) . . ?
C39 C38 C36 121.6(4) . . ?
C37 C38 C36 121.6(4) . . ?
C40 C39 C38 123.4(4) . . ?
C40 C39 H39 118.3 . . ?
C38 C39 H39 118.3 . . ?
C39 C40 C41 117.6(4) . . ?
C39 C40 C43 121.8(4) . . ?
C41 C40 C43 120.6(4) . . ?
C42 C41 C40 121.2(4) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C37 119.3(4) . . ?
C41 C42 C44 120.8(4) . . ?
C37 C42 C44 119.9(4) . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N2 C44 C42 111.9(4) . . ?
N2 C44 H44A 109.2 . . ?
C42 C44 H44A 109.2 . . ?
N2 C44 H44B 109.2 . . ?
C42 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C46 N2 115.5(3) . . ?
C48 C46 H46A 108.4 . . ?
N2 C46 H46A 108.4 . . ?
C48 C46 H46B 108.4 . . ?
N2 C46 H46B 108.4 . . ?
H46A C46 H46B 107.5 . . ?
O6 C47 C48 119.6(3) . . ?
O6 C47 C52 119.9(3) . . ?
C48 C47 C52 120.5(4) . . ?
C49 C48 C47 119.7(4) . . ?
C49 C48 C46 120.0(4) . . ?
C47 C48 C46 120.1(4) . . ?
C48 C49 C50 121.2(4) . . ?
C48 C49 H49 119.4 . . ?
C50 C49 H49 119.4 . . ?
C51 C50 C49 117.5(4) . . ?
C51 C50 C53 122.5(4) . . ?
C49 C50 C53 119.9(4) . . ?
C52 C51 C50 123.3(4) . . ?
C52 C51 H51 118.3 . . ?
C50 C51 H51 118.3 . . ?
C51 C52 C47 117.6(4) . . ?
C51 C52 C54 121.2(3) . . ?
C47 C52 C54 121.2(4) . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C2 C54 C52 115.0(4) . . ?
C2 C54 H54A 108.5 . . ?
C52 C54 H54A 108.5 . . ?
C2 C54 H54B 108.5 . . ?
C52 C54 H54B 108.5 . . ?
H54A C54 H54B 107.5 . . ?
N3 C61 C62 179.6(10) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C64 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N4 C64 C63 178.3(7) . . ?
C19 N1 C18 111.4(3) . . ?
C19 N1 C20 109.7(4) . . ?
C18 N1 C20 113.4(3) . . ?
C19 N1 H1 107.3 . . ?
C18 N1 H1 107.3 . . ?
C20 N1 H1 107.3 . . ?
C45 N2 C44 111.5(3) . . ?
C45 N2 C46 108.9(3) . . ?
C44 N2 C46 112.7(3) . . ?
C45 N2 H2 107.9 . . ?
C44 N2 H2 107.9 . . ?
C46 N2 H2 107.9 . . ?
C1 O1 Ti1 140.9(3) . . ?
C10 O2 H2A 109.5 . . ?
C21 O3 Ti2 142.6(2) . . ?
C29 O4 Ti2 142.8(3) . . ?
C37 O5 H5A 109.5 . . ?
C47 O6 Ti1 143.5(3) . . ?
Ti2 O7 Ti1 172.65(17) . . ?
O7 Ti1 O6 100.63(13) . . ?
O7 Ti1 O1 94.90(12) . . ?
O6 Ti1 O1 99.19(13) . . ?
O7 Ti1 O8 86.50(13) . . ?
O6 Ti1 O8 171.03(13) . . ?
O1 Ti1 O8 85.49(13) . . ?
O7 Ti1 Br2 168.80(9) . . ?
O6 Ti1 Br2 89.29(9) . . ?
O1 Ti1 Br2 88.59(9) . . ?
O8 Ti1 Br2 83.15(9) . . ?
O7 Ti1 Br1 88.29(8) . . ?
O6 Ti1 Br1 91.97(8) . . ?
O1 Ti1 Br1 167.59(10) . . ?
O8 Ti1 Br1 82.74(9) . . ?
Br2 Ti1 Br1 86.14(3) . . ?
O7 Ti2 O3 102.69(12) . . ?
O7 Ti2 O4 96.18(13) . . ?
O3 Ti2 O4 98.50(12) . . ?
O7 Ti2 O9 85.28(12) . . ?
O3 Ti2 O9 169.60(13) . . ?
O4 Ti2 O9 87.11(12) . . ?
O7 Ti2 Br3 164.40(9) . . ?
O3 Ti2 Br3 90.90(9) . . ?
O4 Ti2 Br3 89.25(9) . . ?
O9 Ti2 Br3 80.38(9) . . ?
O7 Ti2 Br4 86.94(9) . . ?
O3 Ti2 Br4 90.06(9) . . ?
O4 Ti2 Br4 169.98(8) . . ?
O9 Ti2 Br4 83.65(9) . . ?
Br3 Ti2 Br4 85.40(3) . . ?
Ti2 O9 H9A 115(4) . . ?
Ti2 O9 H9B 112(4) . . ?
H9A O9 H9B 112(4) . . ?
Ti1 O8 H8C 111(4) . . ?
Ti1 O8 H8D 120(4) . . ?
H8C O8 H8D 102(4) . . ?
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
C1 O1 1.355(5) . ?
C1 C6 1.401(6) . ?
C1 C2 1.402(6) . ?
C2 C3 1.396(6) . ?
C2 C54 1.508(6) . ?
C3 C4 1.382(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(7) . ?
C4 C7 1.511(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 C8 1.511(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C11 1.518(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 O2 1.365(5) . ?
C10 C15 1.377(6) . ?
C10 C11 1.400(6) . ?
C11 C12 1.388(6) . ?
C12 C13 1.395(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(7) . ?
C13 C17 1.525(6) . ?
C14 C15 1.392(6) . ?
C14 H14 0.9500 . ?
C15 C18 1.511(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N1 1.512(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N1 1.485(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.494(6) . ?
C20 N1 1.514(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O3 1.358(5) . ?
C21 C22 1.401(6) . ?
C21 C26 1.404(6) . ?
C22 C23 1.384(6) . ?
C23 C24 1.399(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(6) . ?
C24 C27 1.506(6) . ?
C25 C26 1.385(6) . ?
C25 H25 0.9500 . ?
C26 C28 1.503(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.517(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O4 1.365(5) . ?
C29 C34 1.399(5) . ?
C29 C30 1.406(5) . ?
C30 C31 1.379(6) . ?
C31 C32 1.395(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(6) . ?
C32 C35 1.502(6) . ?
C33 C34 1.386(6) . ?
C33 H33 0.9500 . ?
C34 C36 1.511(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.524(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O5 1.367(5) . ?
C37 C42 1.385(6) . ?
C37 C38 1.403(6) . ?
C38 C39 1.390(6) . ?
C39 C40 1.384(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.398(6) . ?
C40 C43 1.518(6) . ?
C41 C42 1.384(6) . ?
C41 H41 0.9500 . ?
C42 C44 1.507(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N2 1.506(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N2 1.489(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.498(5) . ?
C46 N2 1.515(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O6 1.360(5) . ?
C47 C48 1.393(5) . ?
C47 C52 1.412(5) . ?
C48 C49 1.383(6) . ?
C49 C50 1.400(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.389(6) . ?
C50 C53 1.525(6) . ?
C51 C52 1.380(6) . ?
C51 H51 0.9500 . ?
C52 C54 1.512(6) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C61 N3 1.124(7) . ?
C61 C62 1.441(8) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.442(8) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 N4 1.136(7) . ?
N1 H1 1.0000 . ?
N2 H2 1.0000 . ?
O1 Ti1 1.883(3) . ?
O2 H2A 0.8400 . ?
O3 Ti2 1.825(3) . ?
O4 Ti2 1.869(3) . ?
O5 H5A 0.8400 . ?
O6 Ti1 1.828(3) . ?
O7 Ti2 1.817(3) . ?
O7 Ti1 1.817(3) . ?
Br1 Ti1 2.6748(8) . ?
Br2 Ti1 2.6040(9) . ?
Br3 Ti2 2.5796(9) . ?
Br4 Ti2 2.6647(9) . ?
Ti1 O8 2.134(3) . ?
Ti2 O9 2.152(3) . ?
O9 H9A 0.82(3) . ?
O9 H9B 0.81(3) . ?
O8 H8C 0.83(3) . ?
O8 H8D 0.83(3) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.007 0.000 527 109 ' '
