Bis(2,2'-bipyridine){ethyl 4'-[<i>N</i>-(4-carbamoylphenyl)carbamoyl]-2,2'-bipyridine-4-carboxylate}ruthenium(II) bis[hexafluoridophosphate(V)]
Hirahara, Masanari; Masaoka, Shigeyuki; Sakai, Ken; Acta Crystallographica Section E 65 (2009) m228–m229; doi:10.1107/S1600536809002360

data_2220849
_publ_section_title
;Bis(2,2'-bipyridine){ethyl
 4'-[<i>N</i>-(4-carbamoylphenyl)carbamoyl]-2,2'-bipyridine-4-carboxylate}ruthenium(II)
 bis[hexafluoridophosphate(V)]
;
_journal_coeditor_code           KP2198
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m228
_journal_page_last               m229
_journal_paper_doi               10.1107/S1600536809002360
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ru (C10 H8 N2)2 (C21 H18 N4 O4)] (P F6)2'
_chemical_formula_moiety         'C41 H34 N8 O4 Ru 2+ , 2F6 P -'
_chemical_formula_sum            'C41 H34 F12 N8 O4 P2 Ru'
_chemical_formula_weight         1093.77
_chemical_name_systematic
;
Bis(2,2'-bipyridine){ethyl
4'-[<i>N</i>-(4-carbamoylphenyl)carbamoyl]-2,2'-bipyridine-4-
carboxylate}ruthenium(II) bis[hexafluoridophosphate(V)]
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.344(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.400(3)
_cell_length_b                   13.187(2)
_cell_length_c                   18.863(3)
_cell_measurement_reflns_used    7706
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.19
_cell_volume                     4263.0(12)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'KENX (Sakai, 2004)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), TEXSAN (Molecular Structure Corporation,
2001),
KENX (Sakai, 2004) and ORTEPII (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23329
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.7173
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.479
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0524P)^2^+2.5961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                6405
_reflns_number_total             9357
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2198.cif
_cod_data_source_block           I
_cod_original_cell_volume        4262.9(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220849
_cod_database_fobs_code          2220849