#------------------------------------------------------------------------------
#$Date: 2019-11-17 05:39:56 +0100 (Sun 17 de Nov de 2019) $
#$Revision: 228463 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/25/7122542.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_7122542
loop_
_publ_author_name
'Fedushkin, Igor L.'
'Lukina, Daria A.'
'Skatova, Alexandra A.'
'Lukoyanov, Anton N.'
'Cherkasov, Anton V.'
_publ_section_title
;
 Ca(ii), Yb(ii) and Tm(iii) complexes with tri- and tetra-anions of
 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene.
;
_journal_issue                   92
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12950
_journal_page_last               12953
_journal_paper_doi               10.1039/c8cc08108e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C80 H96 N4 Na2 O2 Tm2'
_chemical_formula_sum            'C80 H96 N4 Na2 O2 Tm2'
_chemical_formula_weight         1529.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-08-02 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.656(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.694(3)
_cell_length_b                   16.730(4)
_cell_length_c                   14.700(3)
_cell_measurement_reflns_used    5163
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.34
_cell_volume                     3366.4(13)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  SHELXL-2017/1
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex (CCD)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.789
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.055
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0468
_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)+(0.0569P)²+5.0548P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6550
_reflns_number_total             8741
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc08108e2.cif
_cod_data_source_block           tmnabian
_cod_depositor_comments
'Adding full bibliography for 7122540--7122542.cif.'
_cod_original_cell_volume        3366.3(13)
_cod_database_code               7122542
_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   0.510
_shelx_estimated_absorpt_t_max   0.878
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Tm1 Tm 0.61476(2) 0.46802(2) 0.36472(2) 0.01548(7) Uani 1 1 d . .
Na1 Na 0.35719(17) 0.57567(13) 0.38985(15) 0.0277(5) Uani 1 1 d . .
O1 O 0.7047(3) 0.4075(2) 0.2529(2) 0.0230(8) Uani 1 1 d . .
N1 N 0.3764(3) 0.6498(2) 0.5709(3) 0.0171(8) Uani 1 1 d . .
N2 N 0.5438(3) 0.5592(2) 0.6544(3) 0.0162(8) Uani 1 1 d . .
C1 C 0.4678(4) 0.6418(3) 0.5274(3) 0.0148(9) Uani 1 1 d . .
C2 C 0.5453(4) 0.5916(3) 0.5637(3) 0.0164(9) Uani 1 1 d . .
C3 C 0.6155(4) 0.5793(3) 0.4950(3) 0.0167(10) Uani 1 1 d . .
C4 C 0.5830(3) 0.6291(3) 0.4185(3) 0.0134(9) Uani 1 1 d . .
C5 C 0.4929(4) 0.6666(3) 0.4379(3) 0.0177(10) Uani 1 1 d . .
C6 C 0.4506(4) 0.7171(3) 0.3692(3) 0.0187(10) Uani 1 1 d . .
H6A H 0.388806 0.741537 0.377243 0.022 Uiso 1 1 calc R U
C7 C 0.5015(4) 0.7295(3) 0.2907(3) 0.0211(11) Uani 1 1 d . .
H7A H 0.474178 0.764407 0.245825 0.025 Uiso 1 1 calc R U
C8 C 0.5916(4) 0.6931(3) 0.2739(3) 0.0212(11) Uani 1 1 d . .
H8A H 0.623657 0.704124 0.218803 0.025 Uiso 1 1 calc R U
C9 C 0.6348(4) 0.6406(3) 0.3380(4) 0.0191(10) Uani 1 1 d . .
C10 C 0.7222(4) 0.5934(3) 0.3304(4) 0.0228(11) Uani 1 1 d . .
H10A H 0.751364 0.586402 0.273097 0.027 Uiso 1 1 calc R U
C11 C 0.7640(4) 0.5574(3) 0.4098(4) 0.0233(11) Uani 1 1 d . .
H11A H 0.829826 0.539705 0.407771 0.028 Uiso 1 1 calc R U
C12 C 0.7149(4) 0.5462(3) 0.4904(4) 0.0195(10) Uani 1 1 d . .
H12A H 0.744311 0.518400 0.540468 0.023 Uiso 1 1 calc R U
C13 C 0.3240(4) 0.7223(3) 0.5560(3) 0.0196(10) Uani 1 1 d . .
C14 C 0.2240(4) 0.7198(3) 0.5280(3) 0.0210(11) Uani 1 1 d . .
C15 C 0.1760(4) 0.7911(3) 0.5047(4) 0.0253(12) Uani 1 1 d . .
H15A H 0.109287 0.789093 0.485151 0.030 Uiso 1 1 calc R U
C16 C 0.2222(4) 0.8639(3) 0.5091(4) 0.0276(12) Uani 1 1 d . .
H16A H 0.189676 0.911212 0.489375 0.033 Uiso 1 1 calc R U
C17 C 0.3169(4) 0.8665(3) 0.5428(4) 0.0256(12) Uani 1 1 d . .
H17A H 0.348363 0.916961 0.548294 0.031 Uiso 1 1 calc R U
C18 C 0.3680(4) 0.7987(3) 0.5689(4) 0.0206(11) Uani 1 1 d . .
C19 C 0.1661(4) 0.6418(3) 0.5232(4) 0.0226(11) Uani 1 1 d . .
H19A H 0.211763 0.597285 0.540416 0.027 Uiso 1 1 calc R U
C20 C 0.1251(5) 0.6248(4) 0.4271(4) 0.0310(13) Uani 1 1 d . .
H20A H 0.178263 0.626259 0.383871 0.046 Uiso 1 1 calc R U
H20B H 0.076300 0.665455 0.410228 0.046 Uiso 1 1 calc R U
H20C H 0.094478 0.571866 0.425579 0.046 Uiso 1 1 calc R U
C21 C 0.0830(4) 0.6417(4) 0.5909(4) 0.0296(13) Uani 1 1 d . .
H21A H 0.110202 0.647864 0.652889 0.044 Uiso 1 1 calc R U
H21B H 0.047299 0.590973 0.586165 0.044 Uiso 1 1 calc R U
H21C H 0.038293 0.686018 0.576907 0.044 Uiso 1 1 calc R U
C22 C 0.4684(4) 0.8088(3) 0.6146(4) 0.0217(11) Uani 1 1 d . .
H22A H 0.493066 0.754613 0.632343 0.026 Uiso 1 1 calc R U
C23 C 0.4611(4) 0.8591(3) 0.7017(4) 0.0256(12) Uani 1 1 d . .
H23A H 0.415112 0.833816 0.742706 0.038 Uiso 1 1 calc R U
H23B H 0.437897 0.912940 0.685933 0.038 Uiso 1 1 calc R U
H23C H 0.525593 0.862737 0.732101 0.038 Uiso 1 1 calc R U
C24 C 0.5421(4) 0.8464(4) 0.5501(4) 0.0271(12) Uani 1 1 d . .
H24A H 0.546909 0.813092 0.495586 0.041 Uiso 1 1 calc R U
H24B H 0.606225 0.849859 0.581150 0.041 Uiso 1 1 calc R U
H24C H 0.519968 0.900064 0.532613 0.041 Uiso 1 1 calc R U
C25 C 0.6312(4) 0.5556(3) 0.7068(3) 0.0156(9) Uani 1 1 d . .
C26 C 0.6381(4) 0.4973(3) 0.7780(3) 0.0184(10) Uani 1 1 d . .
C27 C 0.7285(4) 0.4789(3) 0.8178(4) 0.0233(11) Uani 1 1 d . .
H27A H 0.733212 0.437527 0.861938 0.028 Uiso 1 1 calc R U
C28 C 0.8120(4) 0.5200(3) 0.7940(4) 0.0274(12) Uani 1 1 d . .
H28A H 0.874512 0.503527 0.816618 0.033 Uiso 1 1 calc R U
C29 C 0.8027(4) 0.5852(3) 0.7369(4) 0.0249(11) Uani 1 1 d . .
H29A H 0.858699 0.616832 0.725694 0.030 Uiso 1 1 calc R U
C30 C 0.7135(4) 0.6060(3) 0.6953(3) 0.0196(10) Uani 1 1 d . .
C31 C 0.5447(4) 0.4628(3) 0.8154(3) 0.0219(11) Uani 1 1 d . .
H31A H 0.503184 0.443053 0.763066 0.026 Uiso 1 1 calc R U
C32 C 0.5604(5) 0.3936(3) 0.8827(4) 0.0299(13) Uani 1 1 d . .
H32A H 0.595831 0.350389 0.853104 0.045 Uiso 1 1 calc R U
H32B H 0.496880 0.373825 0.901922 0.045 Uiso 1 1 calc R U
H32C H 0.598394 0.412509 0.935928 0.045 Uiso 1 1 calc R U
C33 C 0.4890(4) 0.5298(4) 0.8631(4) 0.0296(12) Uani 1 1 d . .
H33A H 0.479276 0.574790 0.821110 0.044 Uiso 1 1 calc R U
H33B H 0.526814 0.547685 0.916948 0.044 Uiso 1 1 calc R U
H33C H 0.425398 0.509667 0.881642 0.044 Uiso 1 1 calc R U
C34 C 0.7034(4) 0.6900(3) 0.6548(3) 0.0206(11) Uani 1 1 d . .
H34A H 0.640730 0.692144 0.618197 0.025 Uiso 1 1 calc R U
C35 C 0.6950(4) 0.7480(3) 0.7350(4) 0.0271(12) Uani 1 1 d . .
H35A H 0.686377 0.802539 0.711842 0.041 Uiso 1 1 calc R U
H35B H 0.754548 0.745219 0.773400 0.041 Uiso 1 1 calc R U
H35C H 0.638562 0.733234 0.770957 0.041 Uiso 1 1 calc R U
C36 C 0.7858(5) 0.7149(3) 0.5932(4) 0.0300(13) Uani 1 1 d . .
H36A H 0.773234 0.768854 0.569888 0.045 Uiso 1 1 calc R U
H36B H 0.789315 0.677383 0.542202 0.045 Uiso 1 1 calc R U
H36C H 0.847922 0.714288 0.628099 0.045 Uiso 1 1 calc R U
C37 C 0.6857(5) 0.3250(3) 0.2258(4) 0.0269(12) Uani 1 1 d . .
H37A H 0.616339 0.310944 0.234211 0.032 Uiso 1 1 calc R U
H37B H 0.727384 0.287701 0.261993 0.032 Uiso 1 1 calc R U
C38 C 0.7105(6) 0.3220(4) 0.1267(4) 0.0418(18) Uani 1 1 d . .
H38A H 0.656022 0.342260 0.087380 0.050 Uiso 1 1 calc R U
H38B H 0.727283 0.267019 0.107604 0.050 Uiso 1 1 calc R U
C39 C 0.7987(6) 0.3771(4) 0.1247(4) 0.0441(19) Uani 1 1 d . .
H39A H 0.807586 0.398623 0.062759 0.053 Uiso 1 1 calc R U
H39B H 0.858904 0.348549 0.144681 0.053 Uiso 1 1 calc R U
C40 C 0.7745(5) 0.4435(4) 0.1909(4) 0.0302(13) Uani 1 1 d . .
H40A H 0.834008 0.461677 0.224771 0.036 Uiso 1 1 calc R U
H40B H 0.744906 0.489732 0.158336 0.036 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 0.0033 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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'
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
N1 Tm1 N2 84.92(15) 3_666 3_666
N1 Tm1 O1 83.65(14) 3_666 .
N2 Tm1 O1 110.94(14) 3_666 .
N1 Tm1 C11 111.98(17) 3_666 .
N2 Tm1 C11 154.79(16) 3_666 .
O1 Tm1 C11 90.11(15) . .
N1 Tm1 C10 141.28(17) 3_666 .
N2 Tm1 C10 133.65(16) 3_666 .
O1 Tm1 C10 84.26(14) . .
C11 Tm1 C10 31.54(17) . .
N1 Tm1 C12 97.11(16) 3_666 .
N2 Tm1 C12 132.80(15) 3_666 .
O1 Tm1 C12 116.16(15) . .
C11 Tm1 C12 30.92(16) . .
C10 Tm1 C12 56.66(17) . .
N1 Tm1 C2 61.69(15) 3_666 3_666
N2 Tm1 C2 32.86(14) 3_666 3_666
O1 Tm1 C2 125.42(14) . 3_666
C11 Tm1 C2 140.06(16) . 3_666
C10 Tm1 C2 148.49(15) . 3_666
C12 Tm1 C2 109.25(15) . 3_666
N1 Tm1 C3 108.62(15) 3_666 .
N2 Tm1 C3 102.51(15) 3_666 .
O1 Tm1 C3 145.36(15) . .
C11 Tm1 C3 55.26(16) . .
C10 Tm1 C3 65.74(15) . .
C12 Tm1 C3 32.31(15) . .
C2 Tm1 C3 87.94(14) 3_666 .
N1 Tm1 C1 31.90(15) 3_666 3_666
N2 Tm1 C1 60.73(15) 3_666 3_666
O1 Tm1 C1 111.14(13) . 3_666
C11 Tm1 C1 125.53(16) . 3_666
C10 Tm1 C1 154.98(15) . 3_666
C12 Tm1 C1 98.35(15) . 3_666
C2 Tm1 C1 31.28(15) 3_666 3_666
C3 Tm1 C1 92.66(14) . 3_666
N1 Tm1 C4 137.74(14) 3_666 .
N2 Tm1 C4 94.16(14) 3_666 .
O1 Tm1 C4 134.43(13) . .
C11 Tm1 C4 60.70(15) . .
C10 Tm1 C4 52.15(14) . .
C12 Tm1 C4 54.00(14) . .
C2 Tm1 C4 96.39(14) 3_666 .
C3 Tm1 C4 30.44(14) . .
C1 Tm1 C4 114.31(14) 3_666 .
N1 Tm1 C9 160.41(15) 3_666 .
N2 Tm1 C9 106.24(15) 3_666 .
O1 Tm1 C9 106.37(13) . .
C11 Tm1 C9 52.53(16) . .
C10 Tm1 C9 29.44(15) . .
C12 Tm1 C9 63.44(15) . .
C2 Tm1 C9 120.39(14) 3_666 .
C3 Tm1 C9 53.85(14) . .
C1 Tm1 C9 142.48(14) 3_666 .
C4 Tm1 C9 28.24(13) . .
N1 Tm1 Na1 52.85(11) 3_666 3_666
N2 Tm1 Na1 98.98(11) 3_666 3_666
O1 Tm1 Na1 124.42(10) . 3_666
C11 Tm1 Na1 78.82(13) . 3_666
C10 Tm1 Na1 107.68(12) . 3_666
C12 Tm1 Na1 51.07(12) . 3_666
C2 Tm1 Na1 66.53(11) 3_666 3_666
C3 Tm1 Na1 55.89(11) . 3_666
C1 Tm1 Na1 47.45(11) 3_666 3_666
C4 Tm1 Na1 85.89(10) . 3_666
C9 Tm1 Na1 108.60(11) . 3_666
C5 Na1 C25 127.53(18) . 3_666
C5 Na1 C6 31.48(16) . .
C25 Na1 C6 129.33(18) 3_666 .
C5 Na1 N2 101.63(17) . 3_666
C25 Na1 N2 30.45(14) 3_666 3_666
C6 Na1 N2 117.20(16) . 3_666
C5 Na1 C1 31.44(15) . .
C25 Na1 C1 134.47(18) 3_666 .
C6 Na1 C1 58.33(15) . .
N2 Na1 C1 104.10(15) 3_666 .
C5 Na1 C26 119.25(18) . 3_666
C25 Na1 C26 30.72(15) 3_666 3_666
C6 Na1 C26 105.27(17) . 3_666
N2 Na1 C26 52.68(14) 3_666 3_666
C1 Na1 C26 144.80(18) . 3_666
C5 Na1 C12 121.65(18) . 3_666
C25 Na1 C12 76.47(16) 3_666 3_666
C6 Na1 C12 148.85(17) . 3_666
N2 Na1 C12 75.01(14) 3_666 3_666
C1 Na1 C12 91.55(16) . 3_666
C26 Na1 C12 104.48(16) 3_666 3_666
C5 Na1 N1 55.86(14) . .
C25 Na1 N1 146.94(16) 3_666 .
C6 Na1 N1 72.73(14) . .
N2 Na1 N1 122.26(14) 3_666 .
C1 Na1 N1 28.88(13) . .
C26 Na1 N1 173.41(17) 3_666 .
C12 Na1 N1 76.67(14) 3_666 .
C5 Na1 C3 106.14(17) . 3_666
C25 Na1 C3 65.75(15) 3_666 3_666
C6 Na1 C3 137.58(17) . 3_666
N2 Na1 C3 52.15(13) 3_666 3_666
C1 Na1 C3 83.06(15) . 3_666
C26 Na1 C3 96.44(15) 3_666 3_666
C12 Na1 C3 28.09(13) 3_666 3_666
N1 Na1 C3 81.54(13) . 3_666
C5 Na1 Tm1 77.75(13) . 3_666
C25 Na1 Tm1 110.96(13) 3_666 3_666
C6 Na1 Tm1 104.26(12) . 3_666
N2 Na1 Tm1 91.77(10) 3_666 3_666
C1 Na1 Tm1 46.79(10) . 3_666
C26 Na1 Tm1 141.55(13) 3_666 3_666
C12 Na1 Tm1 44.91(11) 3_666 3_666
N1 Na1 Tm1 36.37(8) . 3_666
C3 Na1 Tm1 45.25(9) 3_666 3_666
C5 Na1 Tm1 69.33(13) . .
C25 Na1 Tm1 60.26(12) 3_666 .
C6 Na1 Tm1 87.84(12) . .
N2 Na1 Tm1 32.33(9) 3_666 .
C1 Na1 Tm1 77.16(12) . .
C26 Na1 Tm1 70.92(12) 3_666 .
C12 Na1 Tm1 93.24(12) 3_666 .
N1 Na1 Tm1 102.59(10) . .
C3 Na1 Tm1 65.27(10) 3_666 .
Tm1 Na1 Tm1 86.20(5) 3_666 .
C37 O1 C40 109.5(4) . .
C37 O1 Tm1 120.9(3) . .
C40 O1 Tm1 129.1(3) . .
C13 N1 C1 117.1(4) . .
C13 N1 Tm1 148.8(3) . 3_666
C1 N1 Tm1 94.1(3) . 3_666
C13 N1 Na1 100.8(3) . .
C1 N1 Na1 67.1(3) . .
Tm1 N1 Na1 90.78(14) 3_666 .
C25 N2 C2 119.3(4) . .
C25 N2 Tm1 150.6(3) . 3_666
C2 N2 Tm1 90.1(3) . 3_666
C25 N2 Na1 70.9(3) . 3_666
C2 N2 Na1 94.0(3) . 3_666
Tm1 N2 Na1 106.90(16) 3_666 3_666
N1 C1 C5 128.4(4) . .
N1 C1 C2 122.3(4) . .
C5 C1 C2 108.4(4) . .
N1 C1 Tm1 54.0(2) . 3_666
C5 C1 Tm1 148.7(3) . 3_666
C2 C1 Tm1 72.7(3) . 3_666
N1 C1 Na1 84.0(3) . .
C5 C1 Na1 65.1(3) . .
C2 C1 Na1 115.2(3) . .
Tm1 C1 Na1 85.77(14) 3_666 .
C3 C2 N2 128.9(4) . .
C3 C2 C1 109.0(4) . .
N2 C2 C1 122.1(4) . .
C3 C2 Tm1 143.7(3) . 3_666
N2 C2 Tm1 57.1(2) . 3_666
C1 C2 Tm1 76.0(3) . 3_666
C2 C3 C4 105.4(4) . .
C2 C3 C12 136.7(5) . .
C4 C3 C12 116.3(4) . .
C2 C3 Tm1 128.2(3) . .
C4 C3 Tm1 81.4(3) . .
C12 C3 Tm1 71.9(3) . .
C2 C3 Na1 78.9(3) . 3_666
C4 C3 Na1 157.5(3) . 3_666
C12 C3 Na1 67.3(3) . 3_666
Tm1 C3 Na1 78.87(12) . 3_666
C9 C4 C5 124.7(4) . .
C9 C4 C3 125.0(4) . .
C5 C4 C3 110.2(4) . .
C9 C4 Tm1 79.1(3) . .
C5 C4 Tm1 127.9(3) . .
C3 C4 Tm1 68.1(3) . .
C4 C5 C6 117.2(4) . .
C4 C5 C1 106.8(4) . .
C6 C5 C1 136.0(5) . .
C4 C5 Na1 108.6(3) . .
C6 C5 Na1 82.9(3) . .
C1 C5 Na1 83.5(3) . .
C7 C6 C5 118.4(5) . .
C7 C6 Na1 118.4(3) . .
C5 C6 Na1 65.6(3) . .
C7 C6 H6A 120.8 . .
C5 C6 H6A 120.8 . .
Na1 C6 H6A 86.4 . .
C6 C7 C8 123.3(5) . .
C6 C7 H7A 118.3 . .
C8 C7 H7A 118.3 . .
C7 C8 C9 120.5(5) . .
C7 C8 H8A 119.8 . .
C9 C8 H8A 119.8 . .
C8 C9 C4 115.8(5) . .
C8 C9 C10 128.7(5) . .
C4 C9 C10 115.4(5) . .
C8 C9 Tm1 131.8(3) . .
C4 C9 Tm1 72.7(3) . .
C10 C9 Tm1 63.3(3) . .
C11 C10 C9 119.0(5) . .
C11 C10 Tm1 73.6(3) . .
C9 C10 Tm1 87.2(3) . .
C11 C10 H10A 120.5 . .
C9 C10 H10A 120.5 . .
Tm1 C10 H10A 109.0 . .
C12 C11 C10 124.3(5) . .
C12 C11 Tm1 75.2(3) . .
C10 C11 Tm1 74.9(3) . .
C12 C11 H11A 117.8 . .
C10 C11 H11A 117.8 . .
Tm1 C11 H11A 123.5 . .
C11 C12 C3 117.2(5) . .
C11 C12 Tm1 73.9(3) . .
C3 C12 Tm1 75.8(3) . .
C11 C12 Na1 142.7(4) . 3_666
C3 C12 Na1 84.6(3) . 3_666
Tm1 C12 Na1 84.02(15) . 3_666
C11 C12 H12A 121.4 . .
C3 C12 H12A 121.4 . .
Tm1 C12 H12A 120.2 . .
Na1 C12 H12A 47.7 3_666 .
C14 C13 N1 119.9(5) . .
C14 C13 C18 117.8(5) . .
N1 C13 C18 122.3(5) . .
C15 C14 C13 119.3(5) . .
C15 C14 C19 118.5(5) . .
C13 C14 C19 122.2(5) . .
C16 C15 C14 122.1(5) . .
C16 C15 H15A 119.0 . .
C14 C15 H15A 119.0 . .
C15 C16 C17 118.3(5) . .
C15 C16 H16A 120.8 . .
C17 C16 H16A 120.8 . .
C16 C17 C18 122.6(5) . .
C16 C17 H17A 118.7 . .
C18 C17 H17A 118.7 . .
C17 C18 C13 119.4(5) . .
C17 C18 C22 118.4(5) . .
C13 C18 C22 122.2(5) . .
C14 C19 C20 112.2(5) . .
C14 C19 C21 111.4(4) . .
C20 C19 C21 109.8(5) . .
C14 C19 H19A 107.8 . .
C20 C19 H19A 107.8 . .
C21 C19 H19A 107.8 . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C18 C22 C24 112.0(4) . .
C18 C22 C23 110.4(4) . .
C24 C22 C23 110.4(4) . .
C18 C22 H22A 108.0 . .
C24 C22 H22A 108.0 . .
C23 C22 H22A 108.0 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
N2 C25 C30 125.0(4) . .
N2 C25 C26 117.9(4) . .
C30 C25 C26 117.1(5) . .
N2 C25 Na1 78.7(3) . 3_666
C30 C25 Na1 111.8(3) . 3_666
C26 C25 Na1 79.8(3) . 3_666
C27 C26 C25 119.9(5) . .
C27 C26 C31 120.8(5) . .
C25 C26 C31 119.0(4) . .
C27 C26 Na1 103.6(3) . 3_666
C25 C26 Na1 69.5(3) . 3_666
C31 C26 Na1 101.4(3) . 3_666
C26 C27 C28 121.0(5) . .
C26 C27 H27A 119.5 . .
C28 C27 H27A 119.5 . .
C29 C28 C27 118.8(5) . .
C29 C28 H28A 120.6 . .
C27 C28 H28A 120.6 . .
C28 C29 C30 121.9(5) . .
C28 C29 H29A 119.0 . .
C30 C29 H29A 119.0 . .
C29 C30 C25 119.1(5) . .
C29 C30 C34 118.0(5) . .
C25 C30 C34 121.9(5) . .
C26 C31 C32 114.7(5) . .
C26 C31 C33 108.8(4) . .
C32 C31 C33 108.6(4) . .
C26 C31 H31A 108.2 . .
C32 C31 H31A 108.2 . .
C33 C31 H31A 108.2 . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C36 C34 C30 114.8(5) . .
C36 C34 C35 110.9(5) . .
C30 C34 C35 106.9(4) . .
C36 C34 H34A 108.0 . .
C30 C34 H34A 108.0 . .
C35 C34 H34A 108.0 . .
C34 C35 H35A 109.5 . .
C34 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C34 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C34 C36 H36A 109.5 . .
C34 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C34 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
O1 C37 C38 104.6(4) . .
O1 C37 H37A 110.8 . .
C38 C37 H37A 110.8 . .
O1 C37 H37B 110.8 . .
C38 C37 H37B 110.8 . .
H37A C37 H37B 108.9 . .
C37 C38 C39 101.5(5) . .
C37 C38 H38A 111.5 . .
C39 C38 H38A 111.5 . .
C37 C38 H38B 111.5 . .
C39 C38 H38B 111.5 . .
H38A C38 H38B 109.3 . .
C38 C39 C40 104.1(5) . .
C38 C39 H39A 110.9 . .
C40 C39 H39A 110.9 . .
C38 C39 H39B 110.9 . .
C40 C39 H39B 110.9 . .
H39A C39 H39B 109.0 . .
O1 C40 C39 104.8(5) . .
O1 C40 H40A 110.8 . .
C39 C40 H40A 110.8 . .
O1 C40 H40B 110.8 . .
C39 C40 H40B 110.8 . .
H40A C40 H40B 108.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 N1 2.188(4) 3_666
Tm1 N2 2.228(4) 3_666
Tm1 O1 2.316(3) .
Tm1 C11 2.602(5) .
Tm1 C10 2.619(5) .
Tm1 C12 2.619(5) .
Tm1 C2 2.654(5) 3_666
Tm1 C3 2.671(5) .
Tm1 C1 2.697(5) 3_666
Tm1 C4 2.846(5) .
Tm1 C9 2.928(5) .
Tm1 Na1 3.690(2) 3_666
Na1 C5 2.488(6) .
Na1 C25 2.623(5) 3_666
Na1 C6 2.710(5) .
Na1 N2 2.722(5) 3_666
Na1 C1 2.726(5) .
Na1 C26 2.755(5) 3_666
Na1 C12 2.886(6) 3_666
Na1 N1 2.942(5) .
Na1 C3 3.114(5) 3_666
O1 C37 1.457(6) .
O1 C40 1.469(6) .
N1 C13 1.422(6) .
N1 C1 1.429(6) .
N2 C25 1.407(6) .
N2 C2 1.440(6) .
C1 C5 1.431(7) .
C1 C2 1.443(7) .
C2 C3 1.429(7) .
C3 C4 1.458(7) .
C3 C12 1.473(7) .
C4 C9 1.411(7) .
C4 C5 1.420(7) .
C5 C6 1.426(7) .
C6 C7 1.381(7) .
C6 H6A 0.9500 .
C7 C8 1.404(8) .
C7 H7A 0.9500 .
C8 C9 1.407(7) .
C8 H8A 0.9500 .
C9 C10 1.441(7) .
C10 C11 1.419(8) .
C10 H10A 0.9500 .
C11 C12 1.392(7) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
C13 C14 1.419(8) .
C13 C18 1.424(7) .
C14 C15 1.400(7) .
C14 C19 1.527(7) .
C15 C16 1.373(8) .
C15 H15A 0.9500 .
C16 C17 1.374(8) .
C16 H16A 0.9500 .
C17 C18 1.382(7) .
C17 H17A 0.9500 .
C18 C22 1.522(8) .
C19 C20 1.533(8) .
C19 C21 1.534(7) .
C19 H19A 1.0000 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 C24 1.538(7) .
C22 C23 1.539(7) .
C22 H22A 1.0000 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 C30 1.423(7) .
C25 C26 1.430(7) .
C26 C27 1.388(7) .
C26 C31 1.521(7) .
C27 C28 1.388(8) .
C27 H27A 0.9500 .
C28 C29 1.380(8) .
C28 H28A 0.9500 .
C29 C30 1.395(7) .
C29 H29A 0.9500 .
C30 C34 1.530(7) .
C31 C32 1.532(7) .
C31 C33 1.537(8) .
C31 H31A 1.0000 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 C36 1.525(8) .
C34 C35 1.533(7) .
C34 H34A 1.0000 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 C38 1.507(8) .
C37 H37A 0.9900 .
C37 H37B 0.9900 .
C38 C39 1.521(11) .
C38 H38A 0.9900 .
C38 H38B 0.9900 .
C39 C40 1.520(8) .
C39 H39A 0.9900 .
C39 H39B 0.9900 .
C40 H40A 0.9900 .
C40 H40B 0.9900 .
