Syntheses, Structures, and Dynamic Behavior of Chiral Racemic Organoantimony and -bismuth Compounds RR'SbCl, RR'BiCl, and RR'SbM [R = 2-(Me2NCH2)C6H4, R' = CH(Me3Si)2, M = H, Li, Na]
Hans J. Breunig; Ioan Ghesner; Mihaiela E. Ghesner; Enno Lork; Inorganic Chemistry 42 (2003) 1751–1757; doi:10.1021/ic026231j

data_4313321
_publ_section_title
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 Syntheses, Structures, and Dynamic Behavior of Chiral Racemic
 Organoantimony and -bismuth Compounds RR'SbCl, RR'BiCl, and RR'SbM [R =
 2-(Me2NCH2)C6H4, R' = CH(Me3Si)2, M = H, Li, Na]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1751
_journal_page_last               1757
_journal_paper_doi               10.1021/ic026231j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C26 H57 N3 Na O Sb Si2'
_chemical_formula_weight         628.67
_chemical_name_systematic
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 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.797(2)
_cell_length_b                   24.991(5)
_cell_length_c                   14.348(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     3499.7(12)
_computing_cell_refinement       'Stoe Cell'
_computing_data_collection       'Stoe Expose'
_computing_data_reduction        'Stoe Reduce'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35477
_diffrn_reflns_theta_full        26.18
_diffrn_reflns_theta_max         26.18
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        'random variation +/-2.0'
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.7762
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Stuart & Walker, Acta Cryst A (1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0057(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1606
_reflns_number_gt                4174
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026231jsi20030107_043210_4.cif
_cod_data_source_block           '[2-(Me2NCH2)C6H4][(Me3Si)2CH]SbNai.tmeda.Et2O'
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'refdelF' changed to 'refdelf'
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 
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_cod_database_code               4313321