The Synthesis and Characterization of Potassium 2,2'-Bipyridinetetranitroruthenate
Daniel A. Freedman; Daron E. Janzen; Kent R. Mann; Inorganic Chemistry 40 (2001) 6009–6016; doi:10.1021/ic010548m

data_4320527
_publ_section_title
;
 The Synthesis and Characterization of Potassium
 2,2'-Bipyridinetetranitroruthenate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6009
_journal_page_last               6016
_journal_paper_doi               10.1021/ic010548m
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C10 H16 K2 N6 O12 Ru'
_chemical_formula_weight         591.56
_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                 99.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8770(15)
_cell_length_b                   12.9271(16)
_cell_length_c                   13.0969(16)
_cell_measurement_temperature    173(2)
_cell_volume                     1981.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10131
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.287
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+9.4970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                3252
_reflns_number_total             3488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010548m_3.cif
_cod_data_source_block           00097
_cod_database_code               4320527