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_4337902
_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         '4(C32 H45 Bi N2 Si), C7'
_chemical_formula_sum            'C135 H180 Bi4 N8 Si4'
_chemical_formula_weight         2863.15
_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             2013-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                108.940(2)
_cell_angle_beta                 93.6783(18)
_cell_angle_gamma                100.2794(18)
_cell_formula_units_Z            1
_cell_length_a                   12.9068(2)
_cell_length_b                   15.6323(4)
_cell_length_c                   17.3240(5)
_cell_measurement_reflns_used    32723
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      37.2900
_cell_measurement_theta_min      3.1700
_cell_volume                     3224.93(14)
_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      120.02(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9486
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0173947000
_diffrn_orient_matrix_UB_12      0.0023846000
_diffrn_orient_matrix_UB_13      -0.0374067000
_diffrn_orient_matrix_UB_21      0.0065963000
_diffrn_orient_matrix_UB_22      0.0488446000
_diffrn_orient_matrix_UB_23      0.0154519000
_diffrn_orient_matrix_UB_31      0.0531788000
_diffrn_orient_matrix_UB_32      0.0041379000
_diffrn_orient_matrix_UB_33      0.0163868000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56171
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1434
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.824
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.104
_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     714
_refine_ls_number_reflns         18799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+2.3857P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15967
_reflns_number_total             18799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500113g_si_002.cif
_cod_data_source_block           (4)
_cod_depositor_comments
'Adding full bibliography for 4337900--4337903.cif.'
_cod_original_cell_volume        3224.91(14)
_cod_database_code               4337902
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Others
 Fixed Sof: C71(0.5) C73(0.5) C74(0.5)
 Fixed Uiso: H1Da(0.032) H1Db(0.032) H1Dc(0.032) H1Ua(0.032) H1Ub(0.032)
 H1Uc(0.032) H3(0.032) H4(0.036) H5(0.031) H7(0.028) H8a(0.057) H8b(0.057)
 H8c(0.057) H9a(0.065) H9b(0.065) H9c(0.065) H10(0.029) H11a(0.061) H11b(0.061)
 H11c(0.061) H12a(0.064) H12b(0.064) H12c(0.064) H15(0.026) H16(0.027)
 H17(0.026) H19(0.024) H20a(0.048) H20b(0.048) H20c(0.048) H21a(0.047)
 H21b(0.047) H21c(0.047) H22(0.034) H23a(0.074) H23b(0.074) H23c(0.074)
 H24a(0.076) H24b(0.076) H24c(0.076) H25a(0.04) H25b(0.04) H25c(0.04)
 H26a(0.047) H26b(0.047) H26c(0.047) H28(0.029) H29(0.036) H30(0.036)
 H31(0.037) H32(0.031) H36(0.025) H37(0.028) H38(0.027) H40(0.021) H41a(0.043)
 H41b(0.043) H41c(0.043) H42a(0.047) H42b(0.047) H42c(0.047) H43(0.025)
 H44a(0.041) H44b(0.041) H44c(0.041) H45a(0.054) H45b(0.054) H45c(0.054)
 H48(0.031) H49(0.037) H50(0.029) H52(0.023) H53a(0.041) H53b(0.041)
 H53c(0.041) H54a(0.042) H54b(0.042) H54c(0.042) H55(0.022) H56a(0.046)
 H56b(0.046) H56c(0.046) H57a(0.047) H57b(0.047) H57c(0.047) H59(0.032)
 H60(0.039) H61(0.039) H62(0.039) H63(0.031)
 Fixed X: H1Da(0.8695) H1Db(0.8861) H1Dc(0.7795) H1Ua(0.664) H1Ub(0.7751)
 H1Uc(0.6938) H3(0.255) H4(0.1988) H5(0.3213) H7(0.5235) H8a(0.3344)
 H8b(0.4348) H8c(0.4401) H9a(0.4253) H9b(0.4384) H9c(0.3305) H10(0.603)
 H11a(0.5396) H11b(0.5753) H11c(0.4543) H12a(0.446) H12b(0.5687) H12c(0.5179)
 H15(1.1276) H16(1.1965) H17(1.0861) H19(0.8558) H20a(0.913) H20b(0.9152)
 H20c(1.0211) H21a(1.0545) H21b(0.9428) H21c(0.9819) H22(0.8064) H23a(0.9774)
 H23b(0.8578) H23c(0.8969) H24a(0.8837) H24b(0.8441) H24c(0.9654) H25a(0.6266)
 H25b(0.7507) H25c(0.6817) H26a(0.7135) H26b(0.7732) H26c(0.6492) H28(0.6317)
 H29(0.6015) H30(0.6239) H31(0.6725) H32(0.7011) H36(0.3406) H37(0.3162)
 H38(0.461) H40(0.5878) H41a(0.4081) H41b(0.4961) H41c(0.5235) H42a(0.4693)
 H42b(0.4648) H42c(0.375) H43(0.7331) H44a(0.6828) H44b(0.736) H44c(0.6121)
 H45a(0.6023) H45b(0.7265) H45c(0.6586) H48(0.9472) H49(1.1213) H50(1.1749)
 H52(0.7399) H53a(0.7944) H53b(0.6916) H53c(0.8023) H54a(0.7711) H54b(0.6602)
 H54c(0.742) H55(1.0211) H56a(1.2334) H56b(1.1969) H56c(1.162) H57a(1.0344)
 H57b(1.1171) H57c(1.1543) H59(0.9747) H60(1.0856) H61(1.0612) H62(0.9261)
 H63(0.8175)
 Fixed Y: H1Da(0.2483) H1Db(0.3548) H1Dc(0.301) H1Ua(0.3784) H1Ub(0.4295)
 H1Uc(0.367) H3(0.7052) H4(0.6196) H5(0.5853) H7(0.7913) H8a(0.7011) H8b(0.756)
 H8c(0.6646) H9a(0.8983) H9b(0.9038) H9c(0.8528) H10(0.6561) H11a(0.499)
 H11b(0.512) H11c(0.4935) H12a(0.64) H12b(0.6595) H12c(0.7344) H15(0.9063)
 H16(0.8544) H17(0.761) H19(0.8714) H20a(0.7471) H20b(0.8264) H20c(0.8126)
 H21a(0.9785) H21b(0.9947) H21c(1.0146) H22(0.6855) H23a(0.5977) H23b(0.5537)
 H23c(0.5722) H24a(0.7918) H24b(0.6919) H24c(0.7295) H25a(0.9452) H25b(0.9698)
 H25c(0.9054) H26a(0.812) H26b(0.9095) H26c(0.8875) H28(0.4933) H29(0.4846)
 H30(0.6186) H31(0.7611) H32(0.7703) H36(0.1111) H37(0.0299) H38(0.0099)
 H40(0.2175) H41a(0.091) H41b(0.1509) H41c(0.0723) H42a(0.3072) H42b(0.2969)
 H42c(0.2377) H43(0.1001) H44a(-0.0588) H44b(-0.0406) H44c(-0.0703)
 H45a(0.0737) H45b(0.1034) H45c(0.1713) H48(0.364) H49(0.4226) H50(0.416)
 H52(0.2542) H53a(0.1567) H53b(0.1879) H53c(0.2341) H54a(0.3911) H54b(0.3428)
 H54c(0.4093) H55(0.3012) H56a(0.3382) H56b(0.2976) H56c(0.2386) H57a(0.462)
 H57b(0.4348) H57c(0.477) H59(0.1492) H60(0.0734) H61(-0.0848) H62(-0.1697)
 H63(-0.0942)
 Fixed Z: H1Da(0.3773) H1Db(0.4252) H1Dc(0.3678) H1Ua(0.5109) H1Ub(0.5625)
 H1Uc(0.5956) H3(0.9229) H4(0.786) H5(0.6963) H7(1.0171) H8a(1.0553)
 H8b(1.1197) H8c(1.0489) H9a(0.9961) H9b(1.0883) H9c(1.0318) H10(0.745)
 H11a(0.7206) H11b(0.6396) H11c(0.6495) H12a(0.6168) H12b(0.6133) H12c(0.6734)
 H15(1.0409) H16(0.9193) H17(0.801) H19(1.0685) H20a(1.0925) H20b(1.1763)
 H20c(1.1392) H21a(1.1542) H21b(1.1786) H21c(1.1011) H22(0.7806) H23a(0.7357)
 H23b(0.7002) H23c(0.7928) H24a(0.7185) H24b(0.654) H24c(0.6866) H25a(0.9883)
 H25b(1.0094) H25c(1.0483) H26a(0.7747) H26b(0.8353) H26c(0.8151) H28(0.9972)
 H29(1.1256) H30(1.2377) H31(1.2223) H32(1.0938) H36(0.446) H37(0.3066)
 H38(0.2373) H40(0.573) H41a(0.5835) H41b(0.6573) H41c(0.5836) H42a(0.5504)
 H42b(0.6372) H42c(0.5645) H43(0.3227) H44a(0.2946) H44b(0.2209) H44c(0.2134)
 H45a(0.1758) H45b(0.1893) H45c(0.2383) H48(0.8337) H49(0.8261) H50(0.7004)
 H52(0.667) H53a(0.7323) H53b(0.7644) H53c(0.8182) H54a(0.8254) H54b(0.7724)
 H54c(0.7436) H55(0.5046) H56a(0.5788) H56b(0.4836) H56c(0.539) H57a(0.5521)
 H57b(0.4909) H57c(0.5859) H59(0.4311) H60(0.3461) H61(0.3049) H62(0.3477)
 H63(0.436)
;