The Metal−NO Interaction in the Redox Systems [Cl5Os(NO)]n-,n= 1−3, andcis-[(bpy)2ClOs(NO)]2+/+: Calculations, Structural, Electrochemical, and Spectroscopic Results
Singh, Priti; Sarkar, Biprajit; Sieger, Monika; Niemeyer, Mark; Fiedler, Jan; Záliš, Stanislav; Kaim, Wolfgang; Inorganic Chemistry 45 (2006) 4602–4609; doi:10.1021/ic0517669

data_4331871
_publ_section_title
;
 The Metal&#x2212;NO Interaction in the Redox Systems [Cl5Os(NO)]n-,n=
 1&#x2212;3, andcis-[(bpy)2ClOs(NO)]2+/+:&#x00A0; Calculations,
 Structural, Electrochemical, and Spectroscopic Results
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4602
_journal_page_last               4609
_journal_paper_doi               10.1021/ic0517669
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C28 H26 Cl2.5 N2.5 O0.5 Os0.5 P'
_chemical_formula_weight         620.21
_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                 98.262(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.50560(10)
_cell_length_b                   19.4011(2)
_cell_length_c                   14.8581(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2711.68(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59472
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.701
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_refine_diff_density_max         0.440
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.581
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.581
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                6160
_reflns_number_total             6695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0517669sup1.cif
_cod_data_source_block           OsNO
_cod_original_cell_volume        2711.68(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C28 H26 Cl2.50 N2.50 O0.50 Os0.50 P'
_cod_database_code               4331871