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_4323475
_publ_section_title
;
 Synthesis and Structures of Intramolecularly Base-Coordinated Group 15
 Aryl Halides
;
_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)2SbCl]'
_chemical_formula_sum            'C21 H27 Cl N2 Sb'
_chemical_formula_weight         464.65
_chemical_name_common            'compound 4'
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                70.614(8)
_cell_angle_beta                 85.738(9)
_cell_angle_gamma                83.094(9)
_cell_formula_units_Z            2
_cell_length_a                   9.1483(11)
_cell_length_b                   9.4868(11)
_cell_length_c                   12.9776(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      20.7
_cell_volume                     1054.0(2)
_computing_cell_refinement       'Enraf CAD4 Express'
_computing_data_collection       'Enraf CAD4 Express'
_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      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       '2\q-\q 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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            9852
_diffrn_reflns_theta_max         34.95
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        6.2
_diffrn_standards_interval_time  1800
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.89859
_exptl_absorpt_correction_T_min  0.37316
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_description       DIAMOND
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0852
_refine_ls_wR_factor_obs         0.0647
_reflns_number_observed          4716
_reflns_number_total             8497
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9701165_1.cif
_cod_data_source_block           smu15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' 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^)+(0.0235P)^2^+0.3228P] 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^)+(0.0235P)^2^+0.3228P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323475