Nonacarbonyl-μ~3~-<i>N</i>,<i>N</i>-diethyldithiocarbamato-κ^3^<i>S</i>:<i>S</i>:<i>S</i>'-μ-hydrido-triosmium(3 <i>Os</i>—<i>Os</i>)
Garcia-Orozco, Ivan; Pastor, Cesar J.; Souto, Beatriz; Delgado, Esther; Hernández, Elisa; Alvarez-Toledano, Cecilio; Acta Crystallographica Section E 61 (2005) m1644–m1645; doi:10.1107/S160053680502338X

data_2206503
_publ_section_title
;Nonacarbonyl-\m~3~-<i>N</i>,<i>N</i>-diethyldithiocarbamato-\k^3^<i>S</i>:<i>S</i>:<i>S</i>'-\m-hydrido-triosmium(3
 <i>Os</i>---<i>Os</i>)
;
_journal_coeditor_code           NG6168
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1644
_journal_page_last               m1645
_journal_paper_doi               10.1107/S160053680502338X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Os3 (C5 H10 N S2) H (C O)9]'
_chemical_formula_moiety         'C14 H11 N O9 Os3 S2'
_chemical_formula_sum            'C14 H11 N O9 Os3 S2'
_chemical_formula_weight         971.96
_chemical_name_systematic
;
Nonacarbonyl-\m~3~N,N-diethyldithiocarbamato-\k^3^S:S:S'-\m-hydrido-
triosmium(3 Os---Os)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.1910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.04120(10)
_cell_length_b                   12.53760(10)
_cell_length_c                   23.2430(2)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6
_cell_measurement_theta_min      3.91
_cell_volume                     4267.53(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31582
_diffrn_reflns_theta_full        67.06
_diffrn_reflns_theta_max         67.06
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    35.264
_exptl_absorpt_correction_T_max  0.494
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.661
_refine_diff_density_min         -2.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.024P)^2^+5.3186P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                7049
_reflns_number_total             7285
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng6168.cif
_cod_data_source_block           I
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206503
_cod_database_fobs_code          2206503