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_7104152
_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         'C33 H41 As I2 N2 , C4 H10 O1'
_chemical_formula_sum            'C37 H51 As I2 N2 O'
_chemical_formula_weight         868.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2004-11-12T18:16:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.267(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2964(3)
_cell_length_b                   24.7180(4)
_cell_length_c                   14.2829(4)
_cell_measurement_reflns_used    132602
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3956.10(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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      0.88453E-1
_diffrn_orient_matrix_UB_12      -0.50734E-2
_diffrn_orient_matrix_UB_13      0.118583E-1
_diffrn_orient_matrix_UB_21      -0.9658E-3
_diffrn_orient_matrix_UB_22      0.99752E-2
_diffrn_orient_matrix_UB_23      0.677513E-1
_diffrn_orient_matrix_UB_31      -0.117906E-1
_diffrn_orient_matrix_UB_32      -0.388777E-1
_diffrn_orient_matrix_UB_33      0.158361E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55518
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.448
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.6052
_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    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.047
_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^)+(0.0339P)^2^+11.8982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                6182
_reflns_number_total             7713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b819723g.txt
_cod_data_source_block           (1)-nov804
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7104152