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_7042268
_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         'C28 H46 Al Bi Cl4 N2 O Si2, C7 H8'
_chemical_formula_sum            'C35 H54 Al Bi Cl4 N2 O Si2'
_chemical_formula_weight         952.74
_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     heavy
_audit_creation_date             2013-08-05
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                87.1030(13)
_cell_angle_beta                 88.7719(13)
_cell_angle_gamma                75.1549(15)
_cell_formula_units_Z            2
_cell_length_a                   10.53512(18)
_cell_length_b                   10.83490(18)
_cell_length_c                   18.5054(3)
_cell_measurement_reflns_used    65467
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      40.9060
_cell_measurement_theta_min      2.8940
_cell_volume                     2039.14(6)
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9807
_diffrn_measurement_details
;
  1 omega   15.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   37.0000 -120.0000 88

  2 omega  -36.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853  -37.0000   60.0000 102

  3 omega  -36.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853  -77.0000    0.0000 109

  4 omega   27.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853  -99.0000  120.0000 54

  5 omega   37.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853 -178.0000   30.0000 91

  6 omega  -99.00  -60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228  -77.0000   30.0000 39

  7 omega  -85.00  -59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228  -57.0000 -120.0000 26

  8 omega -128.00  -94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228 -178.0000   90.0000 34

  9 omega    6.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   77.0000   90.0000 113

 10 omega    6.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   77.0000  150.0000 113

 11 omega   10.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   57.0000  -90.0000 104

 12 omega    6.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   77.0000  -30.0000 113

 13 omega  -71.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228   57.0000 -120.0000 104

 14 omega -131.00  -57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228 -178.0000 -120.0000 74

 15 omega   10.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0853   57.0000   60.0000 104

 16 omega -129.00  -57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228  178.0000 -180.0000 72

 17 omega -129.00  -55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0228  178.0000  -30.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0527368000
_diffrn_orient_matrix_UB_12      0.0241675000
_diffrn_orient_matrix_UB_13      -0.0136749000
_diffrn_orient_matrix_UB_21      0.0454659000
_diffrn_orient_matrix_UB_22      -0.0531605000
_diffrn_orient_matrix_UB_23      0.0166465000
_diffrn_orient_matrix_UB_31      0.0018628000
_diffrn_orient_matrix_UB_32      -0.0344463000
_diffrn_orient_matrix_UB_33      -0.0317632000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73699
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.695
_exptl_absorpt_correction_T_max  0.4429
_exptl_absorpt_correction_T_min  0.3429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0549 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.7742.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         11894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0153
_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^)+(0.0179P)^2^+0.5770P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11491
_reflns_number_total             11894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00230k2.cif
_cod_data_source_block           Compound-3c-55mc2
_cod_depositor_comments
'Adding full bibliography for 7042266--7042269.cif.'
_cod_database_code               7042268
_chemical_oxdiff_formula         c28h46n2o1si2al1cl4bi1
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     40.15
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C23(H23), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C19(H19), C20(H20), C21(H21), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C35(H35A,H35B,H35C)
;