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_7012575
_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 Bi N3 P6 Se6'
_chemical_formula_weight         1427.62
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 120.203(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.300(3)
_cell_length_b                   13.0081(14)
_cell_length_c                   19.672(3)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      4.80
_cell_volume                     5595.3(14)
_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      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        11.36
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.252
_exptl_absorpt_correction_T_max  0.2844
_exptl_absorpt_correction_T_min  0.2339
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.992
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1107
_refine_ls_wR_factor_obs         0.0903
_reflns_number_observed          3002
_reflns_number_total             4880
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b212151d.txt
_cod_data_source_block           Complex_3
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0315P)^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^)+(0.0315P)^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 
;
_cod_original_cell_volume        5595.1(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7012575