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#$Date: 2022-07-01 09:57:13 +0300 (Fri, 01 Jul 2022) $
#$Revision: 276471 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/56/8105600.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_8105600
loop_
_publ_author_name
'Cuihong, Zhang'
'Xiaohu, Wei'
'Liguo, Yang'
'Zhenzhen, He'
'Jiaze, Wu'
'Hao, Liu'
'Xin, Li'
'Zongcheng, Miao'
_publ_section_title
;
 Crystal structure of
 tetrakis(n-butyl)-(μ2-1,2-bis(2-oxidobenzoyl)hydrazine-1,2-diido-κ6
 N,O,O′:N′,O′′,O′′′)ditin(IV),
 C30H44N2O4Sn2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              233
_journal_page_last               234
_journal_paper_doi               10.1515/ncrs-2018-0273
_journal_volume                  234
_journal_year                    2019
_chemical_formula_sum            'C30 H44 N2 O4 Sn2'
_chemical_formula_weight         734.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.0460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8810(8)
_cell_length_b                   16.8999(13)
_cell_length_c                   10.5705(10)
_cell_measurement_reflns_used    1297
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.306
_cell_measurement_theta_min      3.087
_cell_volume                     1585.5(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7943
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_min         2.295
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.8556
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0530P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1637
_reflns_number_total             2782
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0273_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8105600
_shelx_shelxl_version_number     2014/7
_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   0.680
_shelx_estimated_absorpt_t_max   0.856
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Sn1 Sn 0.72189(7) -0.01162(4) 0.43518(5) 0.0693(3) Uani 1 1 d . . . . .
N1 N 0.9354(7) 0.0048(3) 0.5363(6) 0.0582(17) Uani 1 1 d . . . . .
O1 O 1.1006(7) 0.0310(4) 0.6964(5) 0.0813(18) Uani 1 1 d . . . . .
O2 O 0.6280(7) 0.0155(4) 0.6044(5) 0.0804(18) Uani 1 1 d . . . . .
C1 C 0.9675(11) 0.0221(5) 0.6546(8) 0.064(2) Uani 1 1 d . U . . .
C2 C 0.8425(9) 0.0318(5) 0.7442(7) 0.0604(19) Uani 1 1 d . U . . .
C3 C 0.8943(10) 0.0495(5) 0.8696(7) 0.067(2) Uani 1 1 d . U . . .
H3 H 0.9972 0.0533 0.8881 0.081 Uiso 1 1 calc R U . . .
C4 C 0.7939(10) 0.0612(5) 0.9641(8) 0.075(2) Uani 1 1 d . U . . .
H4 H 0.8294 0.0688 1.0470 0.090 Uiso 1 1 calc R U . . .
C5 C 0.6442(11) 0.0617(5) 0.9367(8) 0.074(2) Uani 1 1 d . U . . .
H5 H 0.5768 0.0727 0.9997 0.089 Uiso 1 1 calc R U . . .
C6 C 0.5925(10) 0.0462(5) 0.8166(8) 0.076(2) Uani 1 1 d . U . . .
H6 H 0.4891 0.0460 0.7992 0.091 Uiso 1 1 calc R U . . .
C7 C 0.6888(10) 0.0307(5) 0.7195(7) 0.063(2) Uani 1 1 d . U . . .
C8 C 0.763(2) -0.3159(10) 0.4022(18) 0.248(8) Uani 1 1 d D U . . .
H8A H 0.6814 -0.3104 0.3405 0.372 Uiso 1 1 calc R U . . .
H8B H 0.7785 -0.3709 0.4209 0.372 Uiso 1 1 calc R U . . .
H8C H 0.8528 -0.2938 0.3693 0.372 Uiso 1 1 calc R U . . .
C9 C 0.7244(17) -0.2733(7) 0.5200(16) 0.188(5) Uani 1 1 d D U . . .
H9A H 0.7783 -0.2968 0.5921 0.226 Uiso 1 1 calc R U . . .
H9B H 0.6173 -0.2778 0.5333 0.226 Uiso 1 1 calc R U . . .
C10 C 0.7681(14) -0.1853(7) 0.5085(15) 0.165(5) Uani 1 1 d D U . . .
H10A H 0.7737 -0.1629 0.5930 0.198 Uiso 1 1 calc R U . . .
H10B H 0.8685 -0.1828 0.4755 0.198 Uiso 1 1 calc R U . . .
C11 C 0.6661(12) -0.1330(6) 0.4267(11) 0.119(4) Uani 1 1 d D U . . .
H11A H 0.5632 -0.1395 0.4527 0.143 Uiso 1 1 calc R U . . .
H11B H 0.6703 -0.1505 0.3395 0.143 Uiso 1 1 calc R U . . .
C12 C 0.775(2) 0.2489(9) 0.1736(15) 0.230(7) Uani 1 1 d D U . . .
H12A H 0.8786 0.2369 0.1606 0.346 Uiso 1 1 calc R U . . .
H12B H 0.7546 0.3029 0.1505 0.346 Uiso 1 1 calc R U . . .
H12C H 0.7119 0.2145 0.1221 0.346 Uiso 1 1 calc R U . . .
C13 C 0.7411(17) 0.2367(7) 0.3107(15) 0.174(5) Uani 1 1 d D U . . .
H13A H 0.6339 0.2439 0.3216 0.209 Uiso 1 1 calc R U . . .
H13B H 0.7940 0.2766 0.3611 0.209 Uiso 1 1 calc R U . . .
C14 C 0.7875(14) 0.1546(6) 0.3589(13) 0.151(4) Uani 1 1 d D U . . .
H14A H 0.8747 0.1368 0.3140 0.181 Uiso 1 1 calc R U . . .
H14B H 0.8165 0.1581 0.4481 0.181 Uiso 1 1 calc R U . . .
C15 C 0.6617(11) 0.0941(5) 0.3414(10) 0.100(3) Uani 1 1 d D U . . .
H15A H 0.6435 0.0837 0.2519 0.119 Uiso 1 1 calc R U . . .
H15B H 0.5696 0.1149 0.3753 0.119 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
O2 Sn1 C15 96.7(3) . .
O2 Sn1 C11 98.7(4) . .
C15 Sn1 C11 138.6(4) . .
O2 Sn1 N1 85.2(2) . .
C15 Sn1 N1 109.2(3) . .
C11 Sn1 N1 110.2(3) . .
O2 Sn1 O1 157.2(2) . 3_756
C15 Sn1 O1 90.2(3) . 3_756
C11 Sn1 O1 90.1(4) . 3_756
N1 Sn1 O1 72.0(2) . 3_756
C1 N1 N1 113.1(8) . 3_756
C1 N1 Sn1 131.3(6) . .
N1 N1 Sn1 115.6(6) 3_756 .
C1 O1 Sn1 117.0(5) . 3_756
C7 O2 Sn1 132.2(5) . .
O1 C1 N1 122.3(8) . .
O1 C1 C2 118.4(7) . .
N1 C1 C2 119.3(8) . .
C7 C2 C3 117.7(7) . .
C7 C2 C1 129.1(8) . .
C3 C2 C1 113.0(7) . .
C4 C3 C2 120.7(8) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C5 C4 C3 120.2(8) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 119.7(9) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C5 C6 C7 122.2(9) . .
C5 C6 H6 118.9 . .
C7 C6 H6 118.9 . .
O2 C7 C2 122.6(7) . .
O2 C7 C6 118.1(8) . .
C2 C7 C6 119.3(8) . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C8 C9 C10 109.6(11) . .
C8 C9 H9A 109.8 . .
C10 C9 H9A 109.8 . .
C8 C9 H9B 109.8 . .
C10 C9 H9B 109.8 . .
H9A C9 H9B 108.2 . .
C11 C10 C9 117.5(10) . .
C11 C10 H10A 107.9 . .
C9 C10 H10A 107.9 . .
C11 C10 H10B 107.9 . .
C9 C10 H10B 107.9 . .
H10A C10 H10B 107.2 . .
C10 C11 Sn1 114.1(7) . .
C10 C11 H11A 108.7 . .
Sn1 C11 H11A 108.7 . .
C10 C11 H11B 108.7 . .
Sn1 C11 H11B 108.7 . .
H11A C11 H11B 107.6 . .
C13 C12 H12A 109.5 . .
C13 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C13 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C12 C13 C14 112.6(11) . .
C12 C13 H13A 109.1 . .
C14 C13 H13A 109.1 . .
C12 C13 H13B 109.1 . .
C14 C13 H13B 109.1 . .
H13A C13 H13B 107.8 . .
C15 C14 C13 112.4(9) . .
C15 C14 H14A 109.1 . .
C13 C14 H14A 109.1 . .
C15 C14 H14B 109.1 . .
C13 C14 H14B 109.1 . .
H14A C14 H14B 107.9 . .
C14 C15 Sn1 109.9(7) . .
C14 C15 H15A 109.7 . .
Sn1 C15 H15A 109.7 . .
C14 C15 H15B 109.7 . .
Sn1 C15 H15B 109.7 . .
H15A C15 H15B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O2 2.052(6) .
Sn1 C15 2.103(9) .
Sn1 C11 2.111(10) .
Sn1 N1 2.161(6) .
Sn1 O1 2.164(6) 3_756
N1 C1 1.305(10) .
N1 N1 1.413(12) 3_756
O1 C1 1.256(9) .
O1 Sn1 2.164(6) 3_756
O2 C7 1.338(9) .
C1 C2 1.494(11) .
C2 C7 1.381(11) .
C2 C3 1.419(10) .
C3 C4 1.376(10) .
C3 H3 0.9300 .
C4 C5 1.351(11) .
C4 H4 0.9300 .
C5 C6 1.360(11) .
C5 H5 0.9300 .
C6 C7 1.385(11) .
C6 H6 0.9300 .
C8 C9 1.488(9) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.542(9) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.515(9) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.504(9) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.531(8) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.521(8) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Sn1 O1 C1 N1 -2.5(11) 3_756 . . .
Sn1 O1 C1 C2 177.6(5) 3_756 . . .
N1 N1 C1 O1 1.7(13) 3_756 . . .
Sn1 N1 C1 O1 -178.5(6) . . . .
N1 N1 C1 C2 -178.3(7) 3_756 . . .
Sn1 N1 C1 C2 1.5(12) . . . .
O1 C1 C2 C7 174.8(8) . . . .
N1 C1 C2 C7 -5.1(13) . . . .
O1 C1 C2 C3 -0.7(11) . . . .
N1 C1 C2 C3 179.3(7) . . . .
C7 C2 C3 C4 3.2(13) . . . .
C1 C2 C3 C4 179.3(8) . . . .
C2 C3 C4 C5 -4.9(13) . . . .
C3 C4 C5 C6 3.7(14) . . . .
C4 C5 C6 C7 -0.9(14) . . . .
Sn1 O2 C7 C2 1.2(13) . . . .
Sn1 O2 C7 C6 -179.1(6) . . . .
C3 C2 C7 O2 179.3(8) . . . .
C1 C2 C7 O2 3.9(14) . . . .
C3 C2 C7 C6 -0.4(12) . . . .
C1 C2 C7 C6 -175.8(8) . . . .
C5 C6 C7 O2 179.6(8) . . . .
C5 C6 C7 C2 -0.7(14) . . . .
C8 C9 C10 C11 76.2(18) . . . .
C9 C10 C11 Sn1 173.1(9) . . . .
C12 C13 C14 C15 -89.8(16) . . . .
C13 C14 C15 Sn1 -171.1(9) . . . .
