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_4107834
_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_sum            'C37 H45.88 B22 Br12.12 Cl4 O4 S2'
_chemical_formula_weight         1966.87
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1088(6)
_cell_length_b                   17.7301(7)
_cell_length_c                   27.1659(11)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.30
_cell_volume                     6641.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            90855
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    7.571
_exptl_absorpt_correction_T_max  0.5897
_exptl_absorpt_correction_T_min  0.3983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_meas      0
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         16476
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+3.2812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                10830
_reflns_number_total             16476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710423d-file002.cif
_cod_data_source_block           cr141_0m
_cod_database_code               4107834