Electron-Rich Nitrido-Bridged Complexes. Structure and Bonding in Triosmium Dinitrido Compounds
Claire Newton; Kimberly D. Edwards; Joseph W. Ziller; Nancy M. Doherty; Inorganic Chemistry 38 (1999) 4032–4037; doi:10.1021/ic981257p

data_4322230
_publ_section_title
;
 Electron-Rich Nitrido-Bridged Complexes. Structure and Bonding in
 Triosmium Dinitrido Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4032
_journal_page_last               4037
_journal_paper_doi               10.1021/ic981257p
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C56 H70 Cl8 N8 Os3'
_chemical_formula_weight         1709.40
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 130.958(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.374(3)
_cell_length_b                   12.1153(12)
_cell_length_c                   21.252(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    158
_cell_measurement_theta_max      14.98
_cell_measurement_theta_min      5.09
_cell_volume                     6100.4(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        CARESS
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      158
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         rotating-anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -29
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_diffrn_reflns_theta_max         30.00
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_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 97
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_exptl_absorpt_coefficient_mu    6.627
_exptl_absorpt_correction_T_max  0.6976
_exptl_absorpt_correction_T_min  0.6016
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow/Brown
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_obs          0.0274
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+29.0356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0580
_refine_ls_wR_factor_obs         0.0520
_reflns_number_observed          6920
_reflns_number_total             8898
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981257p_1.cif
_cod_data_source_block           cn4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+29.0356P] 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^)+(0.0194P)^2^+29.0356P] 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        6100.4(10)
_cod_database_code               4322230