Crystal structure of catena-poly[tetrakis(butyl)-μ2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-κ4 O:O,O′,N-μ2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-κ4 O,N,O′:N′-ditin(IV)], C34H50N6O6Sn2
Gao, Zhongjun; Zhang, Haifeng; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 627–629; doi:10.1515/ncrs-2023-0124

data_8107514
_publ_section_title
;
 Crystal structure of
 catena-poly[tetrakis(butyl)-\m2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-\k4
 O:O,O&#x2032;,N-\m2-2-((oxido(phenyl)methylene)hydrazineylidene)propanoato-\k4
 O,N,O&#x2032;:N&#x2032;-ditin(IV)], C34H50N6O6Sn2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              627
_journal_page_last               629
_journal_paper_doi               10.1515/ncrs-2023-0124
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C34 H50 N6 O6 Sn2'
_chemical_formula_sum            'C34 H50 N6 O6 Sn2'
_chemical_formula_weight         876.18
_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   geom
_cell_angle_alpha                79.547(2)
_cell_angle_beta                 82.072(2)
_cell_angle_gamma                87.257(2)
_cell_formula_units_Z            2
_cell_length_a                   12.110(2)
_cell_length_b                   12.406(2)
_cell_length_c                   13.744(3)
_cell_measurement_reflns_used    6347
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.220
_cell_measurement_theta_min      2.354
_cell_volume                     2010.6(6)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10055
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.698
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.8819
_exptl_absorpt_correction_T_min  0.440558
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.0914 before and 0.0254 after correction.
The Ratio of minimum to maximum transmission is 0.4406.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6951
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0471
_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/[\s^2^(Fo^2^)+(0.0652P)^2^+6.1640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5574
_reflns_number_total             6951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0124_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        2010.7(7)
_cod_database_code               8107514
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.698
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H23B-H25C
 2.45 with sigma of 0.01
 H23B-H25A
 1.87 with sigma of 0.02
3. Rigid bond restraints
 C22, C23
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34: within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 3.8A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C31(H31), C32(H32), C33(H33), C34(H34)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              68509
_shelx_hkl_checksum              42650
_olex2_submission_special_instructions 'No special instructions were received'