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_4085429
_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         'C38 H65 N2 Na O3 Si, C4 H8 O'
_chemical_formula_sum            'C42 H73 N2 Na O4 Si'
_chemical_formula_weight         721.10
_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             2015-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                80.126(3)
_cell_angle_beta                 74.202(3)
_cell_angle_gamma                77.259(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3893(4)
_cell_length_b                   12.2039(4)
_cell_length_c                   16.5160(6)
_cell_measurement_reflns_used    9431
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      34.8630
_cell_measurement_theta_min      3.2680
_cell_volume                     2139.28(13)
_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
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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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
  1 omega   78.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608 -178.0000 -150.0000 28

  2 omega   84.00  111.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608  178.0000   60.0000 27

  3 omega  -49.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608  -37.0000  -60.0000 94

  4 omega   -6.00   38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608   77.0000 -120.0000 44

  5 omega   -7.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608   77.0000   90.0000 104

  6 omega  -19.00   16.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1608  -77.0000 -180.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0243562000
_diffrn_orient_matrix_UB_12      -0.0294790000
_diffrn_orient_matrix_UB_13      0.0345163000
_diffrn_orient_matrix_UB_21      -0.0347013000
_diffrn_orient_matrix_UB_22      0.0431087000
_diffrn_orient_matrix_UB_23      0.0254331000
_diffrn_orient_matrix_UB_31      -0.0503724000
_diffrn_orient_matrix_UB_32      -0.0295657000
_diffrn_orient_matrix_UB_33      0.0135021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19499
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.782
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         11706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0568P)^2^+0.7021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9644
_reflns_number_total             11706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5012227_si_002.cif
_cod_data_source_block           55mc12
_cod_depositor_comments
'Adding full bibliography for 4085428--4085431.cif.'
_cod_database_code               4085429
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 91.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H35C)=Sof(H35D)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H40A)=Sof(H40B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C35(H35C,H35D), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C40(H40C,H40D), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'