Synthesis and Characterization of Chelating Triamide Complexes of Bismuth and Antimony
Mark R. Mason; Stanley S. Phulpagar; Mark S. Mashuta; John F. Richardson; Inorganic Chemistry 39 (2000) 3931–3933; doi:10.1021/ic991462k

data_4321291
_publ_contact_author
; Professor Mark R. Mason
  Department of Chemistry 
  University of Toledo
  Toledo, OH 43606, USA
;
_publ_contact_author_email       ' mmason5@uoft02.utoledo.edu'
_publ_contact_author_fax         '(419)530-4033 '
_publ_contact_author_phone       '(419)530-1532 '
_publ_section_title
;
 Synthesis and Characterization of Chelating Triamide Complexes of Bismuth
 and Antimony
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3931
_journal_page_last               3933
_journal_paper_doi               10.1021/ic991462k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C19 H46 Bi N3 Si3'
_chemical_formula_sum            'C19 H46 Bi N3 Si3'
_chemical_formula_weight         609.84
_chemical_name_systematic        ' Bi[N(tBu)SiMe2]3CH'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Oct 5 1995'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record
' Feb_18_2000 text and data added by Mark S. Mashuta'
_cell_angle_alpha                90
_cell_angle_beta                 99.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.158(5)
_cell_length_b                   11.003(5)
_cell_length_c                   22.109(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     2680(2)
_computing_cell_refinement       'Enraf-Nonius Diffractometer Control'
_computing_data_collection       'Enraf-Nonius Diffractometer Control'
_computing_data_reduction        'DIRDIF94 (Beurskens)'
_computing_publication_material  'teXsan (MSC)'
_computing_structure_refinement  'teXsan (MSC)'
_computing_structure_solution    'SIR92 (Altomare)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'data from \w/2\q_scans'
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_source         'normal focus Philips Mo tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5253
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standard_refln_index_l
; -4 4 0
  -2 -2 -13
  -5 0 -4
;
_diffrn_standards_decay_%        'not applied (less than 0.5)'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.723
_exptl_absorpt_correction_T_max  0.133
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       5.9(3)x10^-7^
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'sigma; w=1/\s^2^(F)'
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3507
_reflns_number_total             5004
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ic991462k_1.cif
_cod_data_source_block           mrm06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2679.6(9)
_cod_database_code               4321291