Neutral and cationic bismuth compounds supported by bis(amidodimethyl)disiloxane ligands.
Schwamm, R. J.; Coles, M. P.; Fitchett, C. M.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4066–4074; doi:10.1039/c7dt00230k

data_7042267
_publ_section_title
;
 Neutral and cationic bismuth compounds supported by
 bis(amidodimethyl)disiloxane ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4066
_journal_page_last               4074
_journal_paper_doi               10.1039/c7dt00230k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C60 H90 Bi2 N6 O3 Si6'
_chemical_formula_sum            'C60 H90 Bi2 N6 O3 Si6'
_chemical_formula_weight         1529.87
_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     direct
_audit_creation_date             2014-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                102.811(2)
_cell_angle_beta                 90.9255(19)
_cell_angle_gamma                107.564(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7744(3)
_cell_length_b                   15.3339(4)
_cell_length_c                   19.9763(5)
_cell_measurement_reflns_used    27850
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5190
_cell_measurement_theta_min      3.1080
_cell_volume                     3339.52(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0103533000
_diffrn_orient_matrix_UB_12      -0.0753296000
_diffrn_orient_matrix_UB_13      0.0413621000
_diffrn_orient_matrix_UB_21      0.0959532000
_diffrn_orient_matrix_UB_22      0.0718871000
_diffrn_orient_matrix_UB_23      0.0551053000
_diffrn_orient_matrix_UB_31      -0.0983449000
_diffrn_orient_matrix_UB_32      0.0304627000
_diffrn_orient_matrix_UB_33      0.0394699000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.393
_refine_diff_density_min         -2.520
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         12659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0541P)^2^+1.3429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12247
_reflns_number_total             12659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00230k2.cif
_cod_data_source_block           Compound-2b-55mc33
_cod_depositor_comments
'Adding full bibliography for 7042266--7042269.cif.'
_cod_original_cell_volume        3339.50(16)
_cod_database_code               7042267
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C14H16N5
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.042) H4(0.05) H5(0.046) H7A(0.043) H7B(0.043) H7C(0.043)
 H8A(0.052) H8B(0.052) H8C(0.052) H9A(0.052) H9B(0.052) H9C(0.052) H10A(0.054)
 H10B(0.054) H10C(0.054) H11A(0.062) H11B(0.062) H11C(0.062) H12A(0.05)
 H12B(0.05) H12C(0.05) H15(0.042) H16(0.049) H17(0.048) H19A(0.049) H19B(0.049)
 H19C(0.049) H20A(0.06) H20B(0.06) H20C(0.06) H23(0.03) H24(0.034) H25(0.029)
 H27A(0.039) H27B(0.039) H27C(0.039) H28A(0.035) H28B(0.035) H28C(0.035)
 H29A(0.025) H29B(0.025) H29C(0.025) H30A(0.025) H30B(0.025) H30C(0.025)
 H31A(0.031) H31B(0.031) H31C(0.031) H32A(0.03) H32B(0.03) H32C(0.03)
 H35(0.024) H36(0.03) H37(0.027) H39A(0.028) H39B(0.028) H39C(0.028)
 H40A(0.036) H40B(0.036) H40C(0.036) H43(0.037) H44(0.038) H45(0.033)
 H47A(0.047) H47B(0.047) H47C(0.047) H48A(0.038) H48B(0.038) H48C(0.038)
 H49A(0.044) H49B(0.044) H49C(0.044) H50A(0.044) H50B(0.044) H50C(0.044)
 H51A(0.042) H51B(0.042) H51C(0.042) H52A(0.041) H52B(0.041) H52C(0.041)
 H55(0.039) H56(0.046) H57(0.037) H59A(0.045) H59B(0.045) H59C(0.045)
 H60A(0.036) H60B(0.036) H60C(0.036)
 Fixed X: H3(-0.4689) H4(-0.4513) H5(-0.3834) H7A(-0.3943) H7B(-0.3772) H7C(-
 0.506) H8A(-0.2408) H8B(-0.3708) H8C(-0.3318) H9A(-0.6391) H9B(-0.6147) H9C(-
 0.5397) H10A(-0.4979) H10B(-0.5876) H10C(-0.6126) H11A(-0.4248) H11B(-0.2952)
 H11C(-0.3848) H12A(-0.2707) H12B(-0.2367) H12C(-0.3712) H15(0.1554)
 H16(0.1892) H17(0.0654) H19A(-0.0461) H19B(-0.0507) H19C(0.0725) H20A(-0.0967)
 H20B(-0.2079) H20C(-0.1293) H23(0.3046) H24(0.279) H25(0.0906) H27A(0.1176)
 H27B(0.237) H27C(0.1161) H28A(-0.1618) H28B(-0.1126) H28C(-0.1647) H29A(-
 0.1656) H29B(-0.2358) H29C(-0.1005) H30A(-0.2118) H30B(-0.3068) H30C(-0.259)
 H31A(0.1597) H31B(0.2424) H31C(0.1099) H32A(0.1937) H32B(0.2905) H32C(0.2637)
 H35(-0.2777) H36(-0.2073) H37(-0.0045) H39A(-0.1338) H39B(-0.2539) H39C(-
 0.149) H40A(0.2226) H40B(0.1935) H40C(0.2044) H43(0.5695) H44(0.588)
 H45(0.476) H47A(0.4332) H47B(0.3785) H47C(0.5174) H48A(0.3562) H48B(0.3147)
 H48C(0.241) H49A(0.5008) H49B(0.5009) H49C(0.385) H50A(0.5146) H50B(0.5827)
 H50C(0.5875) H51A(0.2561) H51B(0.1201) H51C(0.2167) H52A(0.1221) H52B(0.085)
 H52C(0.2174) H55(-0.2842) H56(-0.2904) H57(-0.1317) H59A(-0.0646) H59B(-
 0.1998) H59C(-0.1) H60A(0.1509) H60B(0.0761) H60C(0.067)
 Fixed Y: H3(1.067) H4(1.163) H5(1.1227) H7A(0.9497) H7B(0.8664) H7C(0.8725)
 H8A(1.0126) H8B(0.9923) H8C(0.9106) H9A(0.6546) H9B(0.7604) H9C(0.702)
 H10A(0.7726) H10B(0.8065) H10C(0.6988) H11A(0.5619) H11B(0.6147) H11C(0.671)
 H12A(0.5315) H12B(0.5064) H12C(0.477) H15(0.654) H16(0.7274) H17(0.8095)
 H19A(0.5749) H19B(0.6688) H19C(0.6508) H20A(0.899) H20B(0.8079) H20C(0.8298)
 H23(1.049) H24(1.1849) H25(1.1889) H27A(0.826) H27B(0.8874) H27C(0.8648)
 H28A(1.0579) H28B(1.1164) H28C(1.0063) H29A(0.8339) H29B(0.8797) H29C(0.9313)
 H30A(0.6714) H30B(0.7191) H30C(0.6601) H31A(0.9631) H31B(0.9525) H31C(0.948)
 H32A(0.7054) H32B(0.7635) H32C(0.8114) H35(0.7034) H36(0.8269) H37(0.9046)
 H39A(0.649) H39B(0.6171) H39C(0.5783) H40A(0.8424) H40B(0.9149) H40C(0.9345)
 H43(0.9251) H44(0.848) H45(0.6923) H47A(0.928) H47B(0.8335) H47C(0.8816)
 H48A(0.5473) H48B(0.5355) H48C(0.5711) H49A(0.5492) H49B(0.5026) H49C(0.4729)
 H50A(0.7519) H50B(0.6771) H50C(0.7406) H51A(0.3663) H51B(0.3299) H51C(0.3678)
 H52A(0.5626) H52B(0.453) H52C(0.515) H55(0.3391) H56(0.2359) H57(0.2633)
 H59A(0.5537) H59B(0.498) H59C(0.4671) H60A(0.4243) H60B(0.3334) H60C(0.4319)
 Fixed Z: H3(0.257) H4(0.181) H5(0.0759) H7A(0.2928) H7B(0.2365) H7C(0.2491)
 H8A(0.0134) H8B(-0.0193) H8C(-0.0012) H9A(0.1165) H9B(0.1545) H9C(0.1781)
 H10A(-0.0327) H10B(0.0155) H10C(-0.0167) H11A(-0.0971) H11B(-0.1124) H11C(-
 0.0896) H12A(0.0681) H12B(-0.0077) H12C(0.0079) H15(-0.019) H16(-0.1078) H17(-
 0.1323) H19A(0.0547) H19B(0.1037) H19C(0.0919) H20A(-0.055) H20B(-0.0677)
 H20C(-0.1282) H23(0.1957) H24(0.2615) H25(0.2879) H27A(0.168) H27B(0.1461)
 H27C(0.1018) H28A(0.2172) H28B(0.2924) H28C(0.2771) H29A(0.369) H29B(0.3274)
 H29C(0.3528) H30A(0.1685) H30B(0.1982) H30C(0.24) H31A(0.3305) H31B(0.3884)
 H31C(0.4008) H32A(0.2509) H32B(0.3123) H32C(0.2549) H35(0.4777) H36(0.5742)
 H37(0.5957) H39A(0.3358) H39B(0.3697) H39C(0.3833) H40A(0.5151) H40B(0.5755)
 H40C(0.5017) H43(0.564) H44(0.6487) H45(0.6352) H47A(0.4666) H47B(0.4108)
 H47C(0.422) H48A(0.5684) H48B(0.491) H48C(0.5496) H49A(0.428) H49B(0.3497)
 H49C(0.3877) H50A(0.3227) H50B(0.311) H50C(0.3848) H51A(0.2223) H51B(0.2337)
 H51C(0.297) H52A(0.177) H52B(0.1497) H52C(0.1478) H55(0.24) H56(0.3087)
 H57(0.3879) H59A(0.2467) H59B(0.2235) H59C(0.1829) H60A(0.4002) H60B(0.4222)
 H60C(0.4599)
;