Synthesis and properties of spiro-type heterasumanenes containing group 14 elements as bridging atoms
Furukawa, Shunsuke; Hayashi, Keisuke; Yamagishi, Ken; Saito, Masaichi; Materials Chemistry Frontiers 2 (2018) 929–; doi:10.1039/C7QM00590C

data_1553721
_publ_section_title
;
 Synthesis and properties of spiro-type heterasumanenes containing group
 14 elements as bridging atoms
;
_journal_issue                   5
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              929
_journal_paper_doi               10.1039/C7QM00590C
_journal_volume                  2
_journal_year                    2018
_chemical_formula_sum            'C61 H62 Cl2 O12 S4 Sn'
_chemical_formula_weight         1304.93
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2728(7)
_cell_length_b                   21.8232(16)
_cell_length_c                   27.505(2)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.39
_cell_volume                     5523.0(7)
_computing_cell_refinement       'Bruker SAINT (Bruker 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker 2008)'
_computing_data_reduction        'Bruker SAINT and XPREP (Bruker 2008)'
_computing_molecular_graphics    'XSHEL (Bruker, 2002)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31093
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.601
_diffrn_reflns_theta_min         1.195
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP; Bruker AXS 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.985
_exptl_transmission_factor_min   0.969
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         12778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0303P)^2^+5.6639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10316
_reflns_number_total             12778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qm00590c2.cif
_cod_data_source_block           masa1083
_cod_original_cell_volume        5523.1(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1553721
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'SADABS-2008/1 - Bruker AXS 2008'
_shelx_res_checksum              92044