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_4323478
_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         '[(Me2NC10H6)AsCl2]'
_chemical_formula_sum            'C12 H12 As Cl2 N'
_chemical_formula_weight         316.05
_chemical_name_common            'compound 8'
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.713(3)
_cell_length_b                   9.8535(14)
_cell_length_c                   13.310(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     1273.9(5)
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2975
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        3.4
_diffrn_standards_interval_time  1800
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.059
_exptl_absorpt_correction_T_max  0.79791
_exptl_absorpt_correction_T_min  0.19855
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_obs          0.0695
_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^)+(0.1070P)^2^+1.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1819
_refine_ls_wR_factor_obs         0.1588
_reflns_number_observed          1406
_reflns_number_total             1837
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9701165_4.cif
_cod_data_source_block           s14
_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^)+(0.1070P)^2^+1.8441P] 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^)+(0.1070P)^2^+1.8441P] 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        1273.8(5)
_cod_database_code               4323478