Synthesis and Structures of Intramolecularly Base-Coordinated Group 15 Aryl Halides
Claire J. Carmalt; Alan H. Cowley; Robert D. Culp; Richard A. Jones; Smuruthi Kamepalli; Nicholas C. Norman; Inorganic Chemistry 36 (1997) 2770–2776; doi:10.1021/ic9701165

data_4323476
_publ_section_title
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 Synthesis and Structures of Intramolecularly Base-Coordinated Group 15
 Aryl Halides
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2770
_journal_page_last               2776
_journal_paper_doi               10.1021/ic9701165
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         '[(C6H4CH2NMe2)2BiCl]'
_chemical_formula_sum            'C18 H24 Bi Cl N2'
_chemical_formula_weight         512.82
_chemical_name_common            'compound 5'
_chemical_name_systematic
;
?
;
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.536(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9498(10)
_cell_length_b                   11.4695(11)
_cell_length_c                   13.9456(8)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      12.25
_cell_volume                     1850.2(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11673
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        3.4
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    9.672
_exptl_absorpt_correction_T_max  0.50404
_exptl_absorpt_correction_T_min  0.31933
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_obs          0.0375
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0906
_refine_ls_wR_factor_obs         0.0827
_reflns_number_observed          4147
_reflns_number_total             5393
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9701165_2.cif
_cod_data_source_block           c15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0417P)^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^)+(0.0417P)^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 
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_cod_database_code               4323476