Hydrazine Nitrosation of a Metal-Bound Nitric Oxide: Structural Evidence for the Formation of an Ammine Complex
Prakash, Raju; Götz, Andreas W.; Heinemann, Frank W.; Görling, Andreas; Sellmann, Dieter; Inorganic Chemistry 45 (2006) 4661–4667; doi:10.1021/ic060096j

data_4332185
_publ_section_title
;
 Hydrazine Nitrosation of a Metal-Bound Nitric Oxide:&#x00A0; Structural
 Evidence for the Formation of an Ammine Complex
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4661
_journal_page_last               4667
_journal_paper_doi               10.1021/ic060096j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
;
 C110 H89 N3 Ru2 S8 Si4, 1.83(C H2 Cl2), 2.17(C4 H10 O)
;
_chemical_formula_sum            'C120.52 H114.38 Cl3.65 N3 O2.17 Ru2 S8 Si4'
_chemical_formula_weight         2340.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.221(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.336(1)
_cell_length_b                   37.357(6)
_cell_length_c                   17.580(3)
_cell_measurement_reflns_used    367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     10932(3)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 0.70 \% and 150 sec per frame
;
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            90032
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.645
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1373
_refine_ls_number_reflns         21101
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+33.7356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                15814
_reflns_number_total             21101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060096jsup1.cif
_cod_data_source_block           rp0502
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum
;
 C120.52 H114.38 Cl3.65 N3 O2.17 Ru2 S8 Si4
;
_cod_database_code               4332185