Assigning Hapticity to Cyclopentadienyl Derivatives of Antimony and Bismuth
Day, Benjamin M.; Coles, Martyn P.; Organometallics 32 (2013) 4270–; doi:10.1021/om400434f

data_4081093
_publ_section_title
;
 Assigning Hapticity to Cyclopentadienyl Derivatives of Antimony and
 Bismuth
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4270
_journal_paper_doi               10.1021/om400434f
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H45 Bi N2 Si'
_chemical_formula_sum            'C31 H45 Bi N2 Si'
_chemical_formula_weight         682.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-10-07T22:41:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 114.095(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9419(3)
_cell_length_b                   11.0196(2)
_cell_length_c                   18.7499(3)
_cell_measurement_reflns_used    24044
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3195.48(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.379097E-1
_diffrn_orient_matrix_UB_12      -0.474778E-1
_diffrn_orient_matrix_UB_13      0.469702E-1
_diffrn_orient_matrix_UB_21      -0.05194
_diffrn_orient_matrix_UB_22      -0.251167E-1
_diffrn_orient_matrix_UB_23      0.89667E-2
_diffrn_orient_matrix_UB_31      -0.67716E-2
_diffrn_orient_matrix_UB_32      -0.731444E-1
_diffrn_orient_matrix_UB_33      -0.335672E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39476
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.66
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.575
_exptl_absorpt_correction_T_max  0.3665
_exptl_absorpt_correction_T_min  0.2806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                5958
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400434f_si_002.cif
_cod_data_source_block           (2b)-Bi(Me2Si{NAr}2)Cp
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4081093