Mechanism Elucidation of the cis-trans Isomerization of an Azole Ruthenium-Nitrosyl Complex and Its Osmium Counterpart
Anatolie Gavriluta; Gabriel E. Büchel; Leon Freitag; Ghenadie Novitchi; Jean Bernard Tommasino; Erwann Jeanneau; Paul-Steffen Kuhn; Leticia González; Vladimir B. Arion; Dominique Luneau; Inorganic Chemistry 52 (2013) 6260–6272; doi:10.1021/ic4004824

data_4335081
_publ_section_title
;
 Mechanism Elucidation of the cis-trans Isomerization of an Azole
 Ruthenium-Nitrosyl Complex and Its Osmium Counterpart
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6260
_journal_page_last               6272
_journal_paper_doi               10.1021/ic4004824
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C7 H6 Cl4 N3 O Os, C16 H36 N'
_chemical_formula_sum            'C23 H42 Cl4 N4 O Os'
_chemical_formula_weight         722.61
_chemical_name_systematic
; 
Tetrabutylammonium cis-[tetrachlorido-1H-indazole-nitrosyl-osmate]  
;
_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                 100.7569(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   12.35414(12)
_cell_length_b                   52.4121(4)
_cell_length_c                   13.87637(13)
_cell_measurement_reflns_used    97439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.20
_cell_measurement_theta_min      3.24
_cell_volume                     8827.15(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            201647
_diffrn_reflns_theta_full        74.20
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    11.698
_exptl_absorpt_correction_T_max  0.2912
_exptl_absorpt_correction_T_min  0.1443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         17794
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0474P)^2^+23.0121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                16970
_reflns_number_total             17794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004824_si_001_3.cif
_cod_data_source_block           cis-Os
_cod_original_cell_volume        8827.14(14)
_cod_database_code               4335081