Synthesis and Structures of Sb[N(H)(C6H2tBu3)]3 and Bi[N(H)(C6H2tBu3)]3: Implications for the Steric Limits of Supermesityl Substitution
Neil Burford; Charles L. B. Macdonald; Katherine N. Robertson; T. Stanley Cameron; Inorganic Chemistry 35 (1996) 4013–4016; doi:10.1021/ic951532x

data_4323850
_publ_contact_author
; Neil Burford
  Department of Chemistry
  Dalhousie University
  Halifax, Nova Scotia
  Canada, B3H 4J3
;
_publ_contact_author_email       burford@ac.dal.ca
_publ_contact_author_fax         902--494--1310
_publ_contact_author_phone       902--494--3681
_publ_section_title
;
 Synthesis and Structures of Sb[N(H)(C6H2tBu3)]3 and Bi[N(H)(C6H2tBu3)]3:
 Implications for the Steric Limits of Supermesityl Substitution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4013
_journal_page_last               4016
_journal_paper_doi               10.1021/ic951532x
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         Bi[N(H)(C~6~H~2~^t^Bu~3~)]~3~
_chemical_formula_sum            'C54 H90 Bi N3'
_chemical_formula_weight         990.27
_chemical_name_systematic
; 
 Tris(2,4,6--tri--^t^butylphenylamino)bismuth
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 96.50(4)
_cell_angle_gamma                77.40(5)
_cell_formula_units_Z            2
_cell_length_a                   11.511(5)
_cell_length_b                   24.785(15)
_cell_length_c                   9.981(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      7.72
_cell_measurement_theta_min      3.97
_cell_volume                     2741(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection       'MSC/AFC Diffractometer Control Software'
_computing_data_reduction        'MSC/AFC Diffractometer Control Software'
_computing_molecular_graphics    'teXsan-92 (MSC, 1985 and 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_sigmaI/netI    0.1992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
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_diffrn_reflns_theta_max         20.01
_diffrn_reflns_theta_min         2.51
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8149
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            red--orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
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_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
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_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_obs          0.0619
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1964
_refine_ls_wR_factor_obs         0.1502
_reflns_number_observed          2686
_reflns_number_total             5114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951532x_2.cif
_cod_data_source_block           '[kathy.chuck.chuck6]'
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2741.5(24)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4323850