Triorganotin(iv) cation-promoted dimethyl carbonate synthesis from CO2and methanol: solution and solid-state characterization of an unexpected diorganotin(iv)-oxo cluster
Švec, Petr; Cattey, Hélène; Růžičková, Zdeňka; Holub, Josef; Růžička, Aleš; Plasseraud, Laurent; New Journal of Chemistry 42 (2018) 8253–; doi:10.1039/C7NJ05058E

data_7057331
_publ_section_title
;
 Triorganotin(iv) cation-promoted dimethyl carbonate synthesis from CO2and
 methanol: solution and solid-state characterization of an unexpected
 diorganotin(iv)-oxo cluster
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8253
_journal_paper_doi               10.1039/C7NJ05058E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C35 H31 B F15 N O Sn, C3 H7'
_chemical_formula_sum            'C38 H38 B F15 N O Sn'
_chemical_formula_weight         939.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.857(6)
_cell_angle_beta                 105.667(6)
_cell_angle_gamma                94.144(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0570(6)
_cell_length_b                   12.2820(6)
_cell_length_c                   13.6270(12)
_cell_measurement_reflns_used    38020
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      1
_cell_measurement_theta_min      27.5
_cell_volume                     1866.1(2)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38020
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.726
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.1246 before and 0.0316 after correction. The Ratio of minimum to maximum transmission is 0.6284. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8558
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0317P)^2^+2.5266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7609
_reflns_number_total             8558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj05058e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7057329--7057331.cif.'
_cod_database_code               7057331
_shelx_shelxl_version_number     2017/1
_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. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C10(H10A,H10B), C38(H38A,H38B), C15(H15A,
 H15B), C16(H16A,H16B), C11(H11A,H11B), C7(H7A,H7B), C37(H37A,H37B)
3.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C),
 C36(H36A,H36B,H36C)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'