Dioxo- and nitrido-osmium complexes with imidodiphosphinochalcogenido ligands [N(QPR2)2]− (Q = S or Se; R = Ph or Pri)
Zhang, Qian-Feng; Lau, Kwok-Kin; Chim, Joyce L. C.; Wong, Terry K. T.; Wong, Wing-Tak; Williams, Ian D.; Leung, Wa-Hung; Journal of the Chemical Society, Dalton Transactions  (2000) 3027–; doi:10.1039/b003798m

data_7009825
_publ_section_title
;
 Dioxo- and nitrido-osmium complexes with imidodiphosphinochalcogenido
 ligands [N(QPR2)2]&#x2212; (Q&#x2005;=&#x2005;S or Se;
 R&#x2005;=&#x2005;Ph or Pri)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3027
_journal_paper_doi               10.1039/b003798m
_journal_year                    2000
_chemical_formula_sum            'C72 H60 N3 Os P6 S6'
_chemical_formula_weight         1535.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                82.640(10)
_cell_angle_beta                 86.660(10)
_cell_angle_gamma                78.730(10)
_cell_formula_units_Z            2
_cell_length_a                   10.953(2)
_cell_length_b                   14.611(2)
_cell_length_c                   22.038(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3428.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12301
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1550
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         12044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.264
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.4922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                9955
_reflns_number_total             12044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003798m.txt
_cod_data_source_block           '[Os{N(SPPh2)2}3]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3428.3(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009825