Imino-bis(diisopropylphosphine chalcogenide) complexes of arsenic, antimony and bismuth. Synthesis, CVD studies and X-ray structure of M[N(EPiPr2)2]n (E = Se, S; M = As, Sb, Bi)
Crouch, David J.; Helliwell, Madeline; O'Brien, Paul; Park, Jin-Ho; Waters, John; Williams, David J.; Dalton Transactions  (2003) 1500–1504; doi:10.1039/b212151d

data_7012574
_publ_section_title
;
 Imino-bis(diisopropylphosphine chalcogenide) complexes of arsenic,
 antimony and bismuth. Synthesis, CVD studies and X-ray structure of
 M[N(EPiPr2)2]n (E = Se, S; M = As, Sb, Bi)
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1500
_journal_page_last               1504
_journal_paper_doi               10.1039/b212151d
_journal_year                    2003
_chemical_formula_sum            'C36 H84 N3 P6 Sb Se6'
_chemical_formula_weight         1340.39
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.819(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.959(4)
_cell_length_b                   12.9416(17)
_cell_length_c                   19.316(3)
_cell_measurement_reflns_used    5870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.21
_cell_volume                     5413.2(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21220
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.749
_exptl_absorpt_correction_T_max  0.4502
_exptl_absorpt_correction_T_min  0.3831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+5.0793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                5185
_reflns_number_total             5566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212151d.txt
_cod_data_source_block           s1305abs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5413.1(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7012574