beta-Diiminato complexes of arsenic including the formally AsI compound [As3L3] [L = [N(C6H3Pri2-2,6)C(H)]2CPh].
Hitchcock, Peter B; Lappert, Michael F; Li, Gang; Protchenko, Andrey V; Chemical communications (Cambridge, England) 34 (2009) 428–429; doi:10.1039/b819723g

data_7104153
_publ_section_title
;
 beta-Diiminato complexes of arsenic including the formally AsI
 compound [As3L3] [L = [N(C6H3Pri2-2,6)C(H)]2CPh].
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              428
_journal_page_last               429
_journal_paper_doi               10.1039/b819723g
_journal_volume                  34
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C99 H123 As3 N6, 1.5(C6 H14)'
_chemical_formula_sum            'C108 H144 As3 N6'
_chemical_formula_weight         1751.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-12-22T09:47:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.334(2)
_cell_angle_beta                 96.248(1)
_cell_angle_gamma                110.643(2)
_cell_formula_units_Z            2
_cell_length_a                   15.5396(4)
_cell_length_b                   18.7915(4)
_cell_length_c                   19.6985(5)
_cell_measurement_reflns_used    222463
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5177.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.428873E-1
_diffrn_orient_matrix_UB_12      -0.150196E-1
_diffrn_orient_matrix_UB_13      -0.466374E-1
_diffrn_orient_matrix_UB_21      0.554432E-1
_diffrn_orient_matrix_UB_22      0.160169E-1
_diffrn_orient_matrix_UB_23      -0.232556E-1
_diffrn_orient_matrix_UB_31      -0.888E-3
_diffrn_orient_matrix_UB_32      -0.545154E-1
_diffrn_orient_matrix_UB_33      -0.83513E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.09
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67547
_diffrn_reflns_theta_full        26.7
_diffrn_reflns_theta_max         26.7
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.8747
_exptl_absorpt_correction_T_min  0.8069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         20830
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+19.8033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2259
_reflns_number_gt                13637
_reflns_number_total             20830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b819723g.txt
_cod_data_source_block           (2)-dec3204
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104153