Synthesis and Structure of a Hexacoordinate Carbon Compound
Torahiko Yamaguchi; Yohsuke Yamamoto; Daisuke Kinoshita; Kin-ya Akiba; Yun Zhang; Christopher A. Reed; Daisuke Hashizume; Fujiko Iwasaki; Journal of the American Chemical Society 130 (2008) 6894–6895; doi:10.1021/ja710423d

data_4107835
_publ_section_title
;
 Synthesis and Structure of a Hexacoordinate Carbon Compound
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6894
_journal_page_last               6895
_journal_paper_doi               10.1021/ja710423d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
'C33 H30 O4 S2, C H6 B11 Cl6, C H5.9425 B11 Cl6.0575, 2(C H2 Cl2)'
_chemical_formula_sum            'C37 H45.9425 B22 Cl16.0575 O4 S2'
_chemical_formula_weight         1425.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.170(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.755(1)
_cell_length_b                   17.603(1)
_cell_length_c                   26.404(1)
_cell_measurement_reflns_used    536127
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.12
_cell_measurement_theta_min      0.65
_cell_volume                     6225.0(6)
_computing_cell_refinement       SCALEPACK
_computing_data_collection       EXPRESS
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    XD2006
_computing_publication_material  XD2006
_computing_structure_refinement  XD2006
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'MacScience DIP-Labo'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'SPring-8 BL04B2 beamline'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.3282
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            127885
_diffrn_reflns_theta_full        19.12
_diffrn_reflns_theta_max         15.22
_diffrn_reflns_theta_min         0.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.8766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             2859.6
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.13
_refine_diff_density_rms         0.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.8974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1974
_refine_ls_number_reflns         20016
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.01053
_refine_ls_shift/su_mean         0.00023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w2 = 1/[s^2^(Fo^2^) + (0.01 P)^2^ + P]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                20016
_reflns_number_total             26534
_reflns_threshold_expression     I>1.5\s(I)
_cod_data_source_file            ja710423d-file003.cif
_cod_data_source_block           dication
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4107835