Group 1 Complexes of an (Amido-amino)silane and Their Use in the Synthesis of the Bi(III) Amide, Bi(Me2Si{NAr}{N(H)Ar})Cl2(Ar = 2,6-i-Pr2C6H3)
Schwamm, Ryan J.; Coles, Martyn P.; Fitchett, Christopher M.; Organometallics 34 (2015) 2500–; doi:10.1021/om5012227

data_4085431
_publ_section_title
;
 Group 1 Complexes of an (Amido-amino)silane and Their Use in the
 Synthesis of the Bi(III) Amide, Bi(Me2Si{NAr}{N(H)Ar})Cl2(Ar =
 2,6-i-Pr2C6H3)
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2500
_journal_paper_doi               10.1021/om5012227
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H41 Bi Cl2 N2 Si'
_chemical_formula_sum            'C26 H41 Bi Cl2 N2 Si'
_chemical_formula_weight         689.58
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                84.291(2)
_cell_angle_beta                 82.523(2)
_cell_angle_gamma                88.256(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2487(3)
_cell_length_b                   10.3251(3)
_cell_length_c                   15.3742(4)
_cell_measurement_reflns_used    12550
_cell_measurement_temperature    278.87(10)
_cell_measurement_theta_max      37.6890
_cell_measurement_theta_min      3.1750
_cell_volume                     1448.21(7)
_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-1997 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      278.87(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -42.00   42.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.3736  -37.0000  -30.0000 84

  2 omega  -34.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.4674  -77.0000   60.0000 26

  3 omega   -3.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.3736   19.0000  150.0000 109

  4 omega   -1.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.3736   77.0000 -180.0000 47

  5 omega   73.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.3736   77.0000 -180.0000 27

  6 omega   63.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.3736  178.0000 -180.0000 25

  7 omega  -92.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.4674  -77.0000  -90.0000 92

  8 omega  -93.00   -9.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.4674  -77.0000 -180.0000 84

  9 omega -114.00  -81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.4674  178.0000  -60.0000 33
;
_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      -0.0763582000
_diffrn_orient_matrix_UB_12      0.0061535000
_diffrn_orient_matrix_UB_13      0.0121961000
_diffrn_orient_matrix_UB_21      0.0050979000
_diffrn_orient_matrix_UB_22      0.0687405000
_diffrn_orient_matrix_UB_23      -0.0070332000
_diffrn_orient_matrix_UB_31      -0.0113278000
_diffrn_orient_matrix_UB_32      -0.0021832000
_diffrn_orient_matrix_UB_33      -0.0445787000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14856
_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         25.999
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30840
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         3.078
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5415
_reflns_number_total             5696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5012227_si_002.cif
_cod_data_source_block           Compound5-55mc62
_cod_depositor_comments
'Adding full bibliography for 4085428--4085431.cif.'
_cod_original_cell_volume        1448.20(7)
_cod_database_code               4085431
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C26H41N2SI1CL2BI1
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.016) H3(0.024) H4(0.025) H5(0.022) H7(0.022) H8A(0.038)
 H8B(0.038) H8C(0.038) H9A(0.038) H9B(0.038) H9C(0.038) H10(0.022) H11A(0.042)
 H11B(0.042) H11C(0.042) H12A(0.039) H12B(0.039) H12C(0.039) H15(0.032)
 H16(0.042) H17(0.033) H19(0.019) H20A(0.036) H20B(0.036) H20C(0.036)
 H21A(0.032) H21B(0.032) H21C(0.032) H22(0.027) H23A(0.049) H23B(0.049)
 H23C(0.049) H24A(0.059) H24B(0.059) H24C(0.059) H25A(0.034) H25B(0.034)
 H25C(0.034) H26A(0.038) H26B(0.038) H26C(0.038)
 Fixed X: H3(0.3674) H4(0.2935) H5(0.4237) H7(0.69) H8A(0.5249) H8B(0.6874)
 H8C(0.6488) H9A(0.3935) H9B(0.5199) H9C(0.4751) H10(0.7307) H11A(0.5021)
 H11B(0.6207) H11C(0.5029) H12A(0.6909) H12B(0.8129) H12C(0.8167) H15(1.1956)
 H16(1.3129) H17(1.2752) H19(0.9528) H20A(1.0334) H20B(0.911) H20C(0.8893)
 H21A(1.19) H21B(1.1049) H21C(1.2209) H22(1.0228) H23A(1.0719) H23B(1.1167)
 H23C(1.2364) H24A(1.3282) H24B(1.2117) H24C(1.2221) H25A(0.5978) H25B(0.71)
 H25C(0.7462) H26A(0.7722) H26B(0.7451) H26C(0.6198)
 Fixed Y: H3(1.1199) H4(0.9971) H5(0.8126) H7(1.074) H8A(1.2786) H8B(1.2447)
 H8C(1.299) H9A(1.1403) H9B(1.1636) H9C(1.0213) H10(0.6779) H11A(0.5752)
 H11B(0.5093) H11C(0.6037) H12A(0.7479) H12B(0.6524) H12C(0.8006) H15(0.384)
 H16(0.3659) H17(0.5237) H19(0.6358) H20A(0.3762) H20B(0.4587) H20C(0.4131)
 H21A(0.6888) H21B(0.6258) H21C(0.5431) H22(0.7825) H23A(0.6247) H23B(0.764)
 H23C(0.6637) H24A(0.8192) H24B(0.9244) H24C(0.8806) H25A(0.6203) H25B(0.5632)
 H25C(0.5596) H26A(0.9254) H26B(0.7866) H26C(0.8609)
 Fixed Z: H3(0.6889) H4(0.586) H5(0.5492) H7(0.7916) H8A(0.7133) H8B(0.6789)
 H8C(0.7709) H9A(0.8412) H9B(0.8963) H9C(0.8858) H10(0.6449) H11A(0.6576)
 H11B(0.593) H11C(0.5555) H12A(0.4673) H12B(0.4986) H12C(0.5125) H15(0.7443)
 H16(0.8678) H17(0.9656) H19(0.6797) H20A(0.649) H20B(0.6065) H20C(0.7076)
 H21A(0.6143) H21B(0.5479) H21C(0.5962) H22(0.9624) H23A(1.0769) H23B(1.0946)
 H23C(1.0606) H24A(0.934) H24B(0.9643) H24C(0.8689) H25A(0.8206) H25B(0.8831)
 H25C(0.7809) H26A(0.9209) H26B(0.9708) H26C(0.9259)
;