Reaction of [Os(en)2O2]2+ with Photolyzed [Mo(CN)8]4- in Water
R. Kent Murmann; Charles L. Barnes; Inorganic Chemistry 40 (2001) 6514–6517; doi:10.1021/ic010466y

data_4320632
_publ_contact_author_address
;
  Department of Chemistry
  University of Missouri
  Columbia, MO
  65211
;
_publ_contact_author_email       murmannr@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_name
;
  R. Kent Murmann
;
_publ_contact_author_phone       573-882-2826
_publ_section_title
;
 Reaction of [Os(en)2O2]2+ with Photolyzed [Mo(CN)8]4- in Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6514
_journal_page_last               6517
_journal_paper_doi               10.1021/ic010466y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
;
  Tetraphenylarsonium bis(heptacyanomolybdenum(IV)
   -u-oxo-)bis(ethylenediammine)Osmate(VI)
;
_chemical_formula_sum            'C118 H108 As4 Mo2 N18 O11 Os'
_chemical_formula_weight         2635.93
_chemical_name_systematic
;
   Tetraphenylarsonium trans-bis(heptacyanomolybdenum(IV)
   -u-oxo-)bis(ethylenediammine)Osmate(VI)
;
_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                93.501(7)
_cell_angle_beta                 95.994(7)
_cell_angle_gamma                95.638(8)
_cell_formula_units_Z            2
_cell_length_a                   10.978(5)
_cell_length_b                   13.170(5)
_cell_length_c                   40.322(17)
_cell_measurement_reflns_used    26016
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      0.6
_cell_volume                     5755(4)
_computing_cell_refinement       siemans_SMART
_computing_data_collection       siemans_SMART
_computing_data_reduction        siemans_SAINTv4.05
_computing_molecular_graphics    ORTEP3&XSEED
_computing_publication_material  'MS Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  siemans_SMART_CCD
_diffrn_measurement_method       'omega_scan_b/P/b '
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            26016
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  300min
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    2.524
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.4317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      1.54
_exptl_crystal_density_method    flotation
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
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_refine_diff_density_max         1.282
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       <1
_refine_ls_extinction_method     Larson(1970)
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         16365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.600
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+64.1082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                14226
_reflns_number_total             16365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010466y_1.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:
'_symmetry_space_group_number' data item was removed -- it should
have been renamed to '_space_group_IT_number' as specified in the
replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4320632