Low-Coordinate Bismuth Cations.
Schwamm, Ryan J.; Day, Benjamin M.; Coles, Martyn P.; Fitchett, Christopher M.; Inorganic chemistry 53 (2014) 3778–; doi:10.1021/ic500113g

data_4337903
_publ_section_title
;
 Low-Coordinate Bismuth Cations.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3778
_journal_paper_doi               10.1021/ic500113g
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C28 H45 Bi N2 Si'
_chemical_formula_sum            'C28 H45 Bi N2 Si'
_chemical_formula_weight         646.73
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   28.7503(11)
_cell_length_b                   28.7503(11)
_cell_length_c                   9.8541(5)
_cell_measurement_reflns_used    11085
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      31.4430
_cell_measurement_theta_min      3.5770
_cell_volume                     7053.9(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.7863
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0055573000
_diffrn_orient_matrix_UB_12      0.0188236000
_diffrn_orient_matrix_UB_13      -0.0317728000
_diffrn_orient_matrix_UB_21      -0.0255133000
_diffrn_orient_matrix_UB_22      -0.0212010000
_diffrn_orient_matrix_UB_23      -0.0202478000
_diffrn_orient_matrix_UB_31      -0.0113813000
_diffrn_orient_matrix_UB_32      0.0027396000
_diffrn_orient_matrix_UB_33      0.0613164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16452
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.11
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.876
_refine_diff_density_min         -3.129
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5348
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.1289
_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^)+(0.0001P)^2^+568.9560P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2716
_refine_ls_wR_factor_ref         0.2795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4288
_reflns_number_total             5348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500113g_si_002.cif
_cod_data_source_block           (5)
_cod_depositor_comments
'Adding full bibliography for 4337900--4337903.cif.'
_cod_original_cell_volume        7053.9(6)
_cod_database_code               4337903
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c28h45n2si1bi1
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Others
 Fixed Sof: Bi(0.5) Si(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5)
 H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
 Fixed Uiso: H3(0.042) H4(0.055) H5(0.053) H7(0.049) H8A(0.098) H8B(0.098)
 H8C(0.098) H9A(0.08) H9B(0.08) H9C(0.08) H10(0.057) H11A(0.093) H11B(0.093)
 H11C(0.093) H12A(0.075) H12B(0.075) H12C(0.075) H13A(0.045) H13B(0.045)
 H13C(0.045) H14A(0.052) H14B(0.052) H14C(0.052) H15A(0.034) H15B(0.034)
 H16A(0.08) H16B(0.08) H16C(0.08)
 Fixed X: H3(0.317) H4(0.3006) H5(0.3513) H7(0.4261) H8A(0.4159) H8B(0.4302)
 H8C(0.3706) H9A(0.3419) H9B(0.3534) H9C(0.3142) H10(0.4648) H11A(0.472)
 H11B(0.4829) H11C(0.4273) H12A(0.3642) H12B(0.4153) H12C(0.3921) H13A(0.4895)
 H13B(0.4299) H13C(0.4757) H14A(0.441) H14B(0.4007) H14C(0.4517) H15A(0.43)
 H15B(0.4558) H16A(0.3631) H16B(0.3483) H16C(0.3742)
 Fixed Y: H3(0.5224) H4(0.5205) H5(0.501) H7(0.5163) H8A(0.5795) H8B(0.6034)
 H8C(0.5756) H9A(0.4393) H9B(0.4776) H9C(0.4743) H10(0.4898) H11A(0.5678)
 H11B(0.53) H11C(0.5277) H12A(0.4311) H12B(0.4311) H12C(0.4064) H13A(0.3912)
 H13B(0.3779) H13C(0.4245) H14A(0.4358) H14B(0.3911) H14C(0.39) H15A(0.4416)
 H15B(0.4052) H16A(0.3568) H16B(0.3646) H16C(0.3287)
 Fixed Z: H3(-0.0188) H4(0.2138) H5(0.3578) H7(-0.1736) H8A(-0.307) H8B(-0.16)
 H8C(-0.211) H9A(-0.2075) H9B(-0.3317) H9C(-0.2167) H10(0.2855) H11A(0.3999)
 H11B(0.4926) H11C(0.4994) H12A(0.4222) H12B(0.4778) H12C(0.335) H13A(0.1418)
 H13B(0.159) H13C(0.2434) H14A(-0.2029) H14B(-0.1038) H14C(-0.1548) H15A(-
 0.2668) H15B(-0.2858) H16A(-0.3429) H16B(-0.1947) H16C(-0.2211)
;