Spectroelectrochemistry and DFT analysis of a new {RuNO}n redox system with multifrequency EPR suggesting conformational isomerism in the {RuNO}7 state.
Singh, Priti; Fiedler, Jan; Zális, Stanislav; Duboc, Carole; Niemeyer, Mark; Lissner, Falk; Schleid, Thomas; Kaim, Wolfgang; Inorganic chemistry 46 (2007) 9254–9261; doi:10.1021/ic701206a

data_4338960
_publ_section_title
;
 Spectroelectrochemistry and DFT analysis of a new {RuNO}n redox system
 with multifrequency EPR suggesting conformational isomerism in the
 {RuNO}7 state.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9254
_journal_page_last               9261
_journal_paper_doi               10.1021/ic701206a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C23 H17 F18 N8 O P3 Ru'
_chemical_formula_weight         957.43
_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                   14.7169(2)
_cell_length_b                   17.8342(2)
_cell_length_c                   23.8615(2)
_cell_measurement_temperature    100(2)
_cell_volume                     6262.79(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       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  0.1767
_diffrn_reflns_av_sigmaI/netI    0.1072
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57209
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_type
'numerically with the help of the X-SHAPE soft ware by STOE, based on the program HABITUS by W. Herrendorf, Univ. Giessen, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.868
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0868
_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^)+(0.0001P)^2^+42.1481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                5474
_reflns_number_total             7661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701206a-file003.cif
_cod_data_source_block           c:\crystal\x-red\psmai07
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4338960