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_1553719
_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 Ge O12 S4'
_chemical_formula_weight         1258.83
_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
_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                88.2610(10)
_cell_angle_beta                 82.9470(10)
_cell_angle_gamma                86.2480(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7680(7)
_cell_length_b                   11.2196(8)
_cell_length_c                   25.3543(18)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.35
_cell_volume                     2751.0(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.901
_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  0.0213
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            31792
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.631
_diffrn_reflns_theta_min         1.619
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP; Bruker AXS 2008'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       needle
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.991
_exptl_transmission_factor_min   0.979
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         12721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.8546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10954
_reflns_number_total             12721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qm00590c2.cif
_cod_data_source_block           masa1108
_cod_database_code               1553719
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'SADABS-2008/1 - Bruker AXS 2008'
_shelx_res_checksum              75278