Synthesis and characterization of potassium aryl- and alkyl-substituted silylchalcogenolate ligands.
Brown, Jessie L.; Montgomery, Ashley C.; Samaan, Christopher A.; Janicke, Michael T.; Scott, Brian L.; Gaunt, Andrew J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9841–9852; doi:10.1039/c5dt04433b

data_7038535
_publ_section_title
;
 Synthesis and characterization of potassium aryl- and alkyl-substituted
 silylchalcogenolate ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9841
_journal_page_last               9852
_journal_paper_doi               10.1039/c5dt04433b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C30 H47 K O6.5 Se Si'
_chemical_formula_weight         657.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.2187(15)
_cell_length_b                   9.7757(6)
_cell_length_c                   26.2094(15)
_cell_measurement_temperature    100(1)
_cell_volume                     6549.7(7)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            81128
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_correction_T_min  0.4076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         12444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                10686
_reflns_number_total             12444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04433b2.cif
_cod_data_source_block           dq0189s
_cod_depositor_comments
'Adding full bibliography for 7038530--7038536.cif.'
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C30 H47 K O6.50 Se Si'
_cod_database_code               7038535