Synthesis and Structures of Intramolecularly Base-Coordinated Aryl Group 15 Compounds
Smuruthi Kamepalli; Claire J. Carmalt; Robert D. Culp; Alan H. Cowley; Richard A. Jones; Nicholas C. Norman; Inorganic Chemistry 35 (1996) 6179–6183; doi:10.1021/ic960516c

data_4323946
_publ_section_title
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 Synthesis and Structures of Intramolecularly Base-Coordinated Aryl Group
 15 Compounds
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6179
_journal_page_last               6183
_journal_paper_doi               10.1021/ic960516c
_journal_volume                  35
_journal_year                    1996
_chemical_formula_structural     '((C H3)2 N C10 H6)3 As'
_chemical_formula_sum            'C36 H36 As N3'
_chemical_formula_weight         585.60
_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                 100.708(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5744(12)
_cell_length_b                   16.273(2)
_cell_length_c                   18.884(3)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      11.75
_cell_measurement_theta_min      9.20
_cell_volume                     2891.0(7)
_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      193(2)
_diffrn_measurement_device       'Siemens P3'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10341
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        '0.9414 < d < 1.000'
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.91417
_exptl_absorpt_correction_T_min  0.53076
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.004
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_obs          0.0495
_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^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0982
_refine_ls_wR_factor_obs         0.0815
_reflns_number_observed          4193
_reflns_number_total             6647
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960516c_4.cif
_cod_data_source_block           Compound7
_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^)+(0.0334P)^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^)+(0.0334P)^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_original_cell_volume        2890.9(7)
_cod_database_code               4323946