Cyclometalated [Os(C~N)x(N~N)3-x]^m+^ Mimetics of Tris(2,2'-bipyridine)osmium(II): Covering a 2 V Potencial Range by knwon (x = 0,1) and new (x = 3) species (C~N = o-2-phenylpiriinato)
Ricardo Ceron-Camacho; Simon Hernandez; Ronan Le Lagadec; Alexander D. Ryabov; Chem.Commun. 47 (2011) 2823–; doi:10.1039/c0cc04582a

data_7106040
_publ_section_title
;
 Cyclometalated [Os(C~N)x(N~N)3-x]^m+^ Mimetics of
 Tris(2,2'-bipyridine)osmium(II): Covering a 2 V Potencial Range by knwon
 (x = 0,1) and new (x = 3) species (C~N = o-2-phenylpiriinato)
;
_journal_name_full               Chem.Commun.
_journal_page_first              2823
_journal_paper_doi               10.1039/c0cc04582a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C32 H24 N4 Os, F6 P'
_chemical_formula_sum            'C32 H24 F6 N4 Os P'
_chemical_formula_weight         799.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.0431(9)
_cell_length_b                   15.8867(13)
_cell_length_c                   33.671(3)
_cell_measurement_reflns_used    8095
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.21
_cell_volume                     5907.2(9)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23A (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX AXS CCD area detector'
_diffrn_measurement_method       'omega 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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            46381
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    4.439
_exptl_absorpt_correction_T_max  0.7572
_exptl_absorpt_correction_T_min  0.3684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, Sheldrick, G. M. (1996)'
_exptl_crystal_colour            BLack
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s\^2\^(Fo\^2\^)+(0.0678P)\^2\^] where P=(Fo\^2\^+2Fc\^2\^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                3647
_reflns_number_total             5422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04582A.TXT
_cod_data_source_block           compound-1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_cell_volume        5907.2(8)
_cod_database_code               7106040
_solved_by                       'Simon Hernandez-Ortega'