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_4337901
_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         'C52 H80 Bi2 Cl N4 Si2, C6 H14, Cl4 Ga'
_chemical_formula_sum            'C58 H94 Bi2 Cl5 Ga N4 Si2'
_chemical_formula_weight         1568.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-08-14
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                117.739(4)
_cell_angle_beta                 92.142(3)
_cell_angle_gamma                90.447(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8472(5)
_cell_length_b                   17.0713(7)
_cell_length_c                   17.4081(7)
_cell_measurement_reflns_used    11261
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.5420
_cell_measurement_theta_min      3.4250
_cell_volume                     3375.4(3)
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9682
_diffrn_measurement_details
;
  1 omega -114.00   -8.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -77.0000  -60.0000 106

  2 omega  -95.00   -5.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  125.0000   90.0000 90

  3 omega  -58.00   33.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563   57.0000   60.0000 91

  4 omega   35.00   64.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6563 -125.0000  -60.0000 29

  5 omega  -48.00   10.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000   30.0000 58

  6 omega -125.00  -74.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000   90.0000 51

  7 omega   36.00  109.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  -60.0000 73

  8 omega   46.00  161.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   15.0000    0.0000 115

  9 omega   30.00   82.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   90.0000 52

 10 omega   32.00   91.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   30.0000 59

 11 omega   47.00   93.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 46

 12 omega   24.00  108.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000 -150.0000 84

 13 omega  133.00  178.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000  -90.0000 45

 14 omega   31.00   89.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 58

 15 omega   89.00  159.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000 -120.0000 70

 16 omega   92.00  122.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000  -60.0000 30

 17 omega   55.00  121.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  150.0000 66

 18 omega  141.00  177.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000 -180.0000 36

 19 omega   43.00   99.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  -90.0000 56

 20 omega -114.00  -61.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -57.0000 -180.0000 53

 21 omega -114.00  -10.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563  -57.0000   60.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0882938000
_diffrn_orient_matrix_UB_12      -0.0487052000
_diffrn_orient_matrix_UB_13      0.0196219000
_diffrn_orient_matrix_UB_21      0.0806290000
_diffrn_orient_matrix_UB_22      -0.0580607000
_diffrn_orient_matrix_UB_23      0.0155413000
_diffrn_orient_matrix_UB_31      0.0106908000
_diffrn_orient_matrix_UB_32      0.0682722000
_diffrn_orient_matrix_UB_33      0.0969145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26092
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.996
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48128
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.656
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         13265
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+3.9681P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11200
_reflns_number_total             13265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500113g_si_002.cif
_cod_data_source_block           (3b)
_cod_depositor_comments
'Adding full bibliography for 4337900--4337903.cif.'
_cod_database_code               4337901
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.049) H4(0.055) H5(0.049) H7(0.044) H8A(0.073) H8B(0.073)
 H8C(0.073) H9A(0.073) H9B(0.073) H9C(0.073) H10(0.045) H11A(0.075) H11B(0.075)
 H11C(0.075) H12A(0.078) H12B(0.078) H12C(0.078) H15(0.047) H16(0.045)
 H17(0.043) H19(0.046) H20A(0.08) H20B(0.08) H20C(0.08) H21A(0.08) H21B(0.08)
 H21C(0.08) H22(0.037) H23A(0.081) H23B(0.081) H23C(0.081) H24A(0.062)
 H24B(0.062) H24C(0.062) H25A(0.062) H25B(0.062) H25C(0.062) H26A(0.067)
 H26B(0.067) H26C(0.067) H29(0.041) H30(0.045) H31(0.041) H33(0.042) H34A(0.07)
 H34B(0.07) H34C(0.07) H35A(0.078) H35B(0.078) H35C(0.078) H36(0.041)
 H37A(0.092) H37B(0.092) H37C(0.092) H38A(0.078) H38B(0.078) H38C(0.078)
 H41(0.043) H42(0.05) H43(0.046) H45(0.038) H46A(0.059) H46B(0.059) H46C(0.059)
 H47A(0.069) H47B(0.069) H47C(0.069) H48(0.05) H49A(0.083) H49B(0.083)
 H49C(0.083) H50A(0.082) H50B(0.082) H50C(0.082) H51A(0.075) H51B(0.075)
 H51C(0.075) H52A(0.074) H52B(0.074) H52C(0.074) H60A(0.213) H60B(0.213)
 H60C(0.213) H64A(0.162) H64B(0.162) H65A(0.205) H65B(0.205) H65C(0.205)
 H62A(0.2) H62B(0.2) H63A(0.275) H63B(0.275) H61A(0.352) H61B(0.352)
 Fixed X: H3(-0.1651) H4(-0.3032) H5(-0.2944) H7(0.0774) H8A(-0.0065)
 H8B(0.1066) H8C(0.0766) H9A(-0.0351) H9B(0.0409) H9C(-0.0745) H10(-0.0875)
 H11A(-0.1001) H11B(-0.1472) H11C(-0.2212) H12A(-0.3074) H12B(-0.2383) H12C(-
 0.2425) H15(0.3216) H16(0.4874) H17(0.518) H19(0.0936) H20A(0.1114)
 H20B(0.0316) H20C(0.1446) H21A(0.1774) H21B(0.0634) H21C(0.1578) H22(0.3316)
 H23A(0.462) H23B(0.4907) H23C(0.5444) H24A(0.4869) H24B(0.4318) H24C(0.3683)
 H25A(0.2408) H25B(0.2832) H25C(0.1839) H26A(0.0652) H26B(0.0941) H26C(0.1813)
 H29(0.6951) H30(0.7062) H31(0.56) H33(0.4682) H34A(0.6448) H34B(0.5688)
 H34C(0.5296) H35A(0.5867) H35B(0.6034) H35C(0.6801) H36(0.3043) H37A(0.3315)
 H37B(0.2794) H37C(0.3988) H38A(0.4319) H38B(0.3131) H38C(0.3946) H41(-0.1169)
 H42(-0.0661) H43(0.0998) H45(0.0425) H46A(-0.1297) H46B(-0.0953) H46C(-0.0224)
 H47A(-0.0568) H47B(-0.1079) H47C(-0.1541) H48(0.3054) H49A(0.2282)
 H49B(0.3204) H49C(0.2051) H50A(0.2694) H50B(0.379) H50C(0.3085) H51A(0.3989)
 H51B(0.3934) H51C(0.305) H52A(0.1527) H52B(0.2506) H52C(0.1705) H60A(-0.2659)
 H60B(-0.3044) H60C(-0.2685) H64A(-0.6309) H64B(-0.5454) H65A(-0.4313) H65B(-
 0.4881) H65C(-0.534) H62A(-0.3821) H62B(-0.409) H63A(-0.5826) H63B(-0.5462)
 H61A(-0.4442) H61B(-0.4372)
 Fixed Y: H3(0.5367) H4(0.5096) H5(0.3997) H7(0.4291) H8A(0.5989) H8B(0.5739)
 H8C(0.5779) H9A(0.3748) H9B(0.4476) H9C(0.4705) H10(0.2533) H11A(0.3672)
 H11B(0.2767) H11C(0.3509) H12A(0.2515) H12B(0.1736) H12C(0.1986) H15(0.0471)
 H16(0.0644) H17(0.1578) H19(0.1527) H20A(0.0123) H20B(0.0078) H20C(-0.0266)
 H21A(0.0735) H21B(0.107) H21C(0.1751) H22(0.2894) H23A(0.3609) H23B(0.3634)
 H23C(0.2962) H24A(0.1726) H24B(0.24) H24C(0.1591) H25A(0.431) H25B(0.4366)
 H25C(0.4884) H26A(0.3018) H26B(0.4032) H26C(0.3343) H29(0.2726) H30(0.4055)
 H31(0.4897) H33(0.1719) H34A(0.1228) H34B(0.0556) H34C(0.1098) H35A(0.2327)
 H35B(0.1308) H35C(0.1989) H36(0.4324) H37A(0.4212) H37B(0.5111) H37C(0.5094)
 H38A(0.5878) H38B(0.5834) H38C(0.5407) H41(0.2107) H42(0.1177) H43(0.0621)
 H45(0.2979) H46A(0.1784) H46B(0.2434) H46C(0.167) H47A(0.3821) H47B(0.3793)
 H47C(0.3197) H48(0.1248) H49A(0.0015) H49B(-0.0299) H49C(-0.0426) H50A(0.0372)
 H50B(0.0606) H50C(0.1363) H51A(0.2583) H51B(0.3613) H51C(0.2998) H52A(0.4119)
 H52B(0.466) H52C(0.4245) H60A(0.1536) H60B(0.1302) H60C(0.2275) H64A(0.3521)
 H64B(0.2974) H65A(0.4031) H65B(0.4486) H65C(0.4542) H62A(0.3176) H62B(0.248)
 H63A(0.2461) H63B(0.3374) H61A(0.2063) H61B(0.1403)
 Fixed Z: H3(0.2764) H4(0.3413) H5(0.3825) H7(0.2337) H8A(0.2844) H8B(0.2519)
 H8C(0.3401) H9A(0.1094) H9B(0.1103) H9C(0.137) H10(0.3512) H11A(0.496)
 H11B(0.4831) H11C(0.4869) H12A(0.3466) H12B(0.3404) H12C(0.2644) H15(0.3632)
 H16(0.3259) H17(0.2669) H19(0.3405) H20A(0.2184) H20B(0.2823) H20C(0.281)
 H21A(0.4392) H21B(0.4445) H21C(0.4776) H22(0.227) H23A(0.3355) H23B(0.2499)
 H23C(0.2757) H24A(0.1305) H24B(0.106) H24C(0.1014) H25A(0.3191) H25B(0.4072)
 H25C(0.4049) H26A(0.4558) H26B(0.5007) H26C(0.485) H29(-0.0033) H30(0.123)
 H31(0.1717) H33(-0.137) H34A(-0.0682) H34B(-0.1428) H34C(-0.0486) H35A(-
 0.1955) H35B(-0.2327) H35C(-0.1593) H36(0.0726) H37A(0.1988) H37B(0.2193)
 H37C(0.2402) H38A(0.149) H38B(0.1226) H38C(0.0507) H41(-0.2671) H42(-0.4062)
 H43(-0.4259) H45(-0.0739) H46A(-0.1225) H46B(-0.0258) H46C(-0.0834) H47A(-
 0.1235) H47B(-0.0444) H47C(-0.139) H48(-0.2662) H49A(-0.2659) H49B(-0.3291)
 H49C(-0.3666) H50A(-0.4482) H50B(-0.3991) H50C(-0.3965) H51A(-0.2321) H51B(-
 0.1938) H51C(-0.2591) H52A(-0.1206) H52B(-0.0635) H52C(-0.0259) H60A(-0.4548)
 H60B(-0.3833) H60C(-0.3581) H64A(-0.4778) H64B(-0.5414) H65A(-0.4824) H65B(-
 0.3946) H65C(-0.4766) H62A(-0.403) H62B(-0.4995) H63A(-0.4484) H63B(-0.3704)
 H61A(-0.3665) H61B(-0.4648)
;