Bis(2,2'-bipyridine)[1,9-bis(diphenylphosphanyl)-1,2,3,4,6,7,8,9-octahydropyrimido[1,2-<i>a</i>]pyrimidin-5-ium]ruthenium(II) hexafluoridophosphate dibromide dichloromethane disolvate monohydrate
Shang, Congcong; Vendier, Laure; Sutra, Pierre; Igau, Alain; Acta Crystallographica Section E 69 (2013) m640–m641; doi:10.1107/S1600536813029462

data_2238928
_publ_section_title
;
 Bis(2,2'-bipyridine)[1,9-bis(diphenylphosphanyl)-1,2,3,4,6,7,8,9-octahydropyrimido[1,2-<i>a</i>]pyrimidin-5-ium]ruthenium(II)
 hexafluoridophosphate dibromide dichloromethane disolvate monohydrate
;
_journal_coeditor_code           SU2644
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m640
_journal_page_last               m641
_journal_paper_doi               10.1107/S1600536813029462
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Ru (C31 H32 N3 P2) (C10 H8 N2)2] (P F6) Br2, 2C H2 Cl2, H2 O'
_chemical_formula_moiety
'C51 H48 N7 P2 Ru 3+, P F6 -, 2Br -, 2(C H2 Cl2), H2 O'
_chemical_formula_sum            'C53 H54 Br2 Cl4 F6 N7 O P3 Ru'
_chemical_formula_weight         1414.63
_chemical_name_systematic
;Bis(2,2'-bipyridine)[1,9-bis(diphenylphosphanyl)-1,2,3,4,6,7,8,9-octahydropyrimido[1,2-<i>a</i>]pyrimidin-5-ium]ruthenium(II)
hexafluoridophosphate dibromide dichloromethane
disolvate monohydrate
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.654(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1770(4)
_cell_length_b                   20.9840(5)
_cell_length_c                   16.6730(4)
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3249
_cell_measurement_theta_min      2.9064
_cell_volume                     5621.7(2)
_computing_cell_refinement       'CrysAlis Pro (Agilent, 2012)'
_computing_data_collection       'CrysAlis Pro (Agilent, 2012)'
_computing_data_reduction        'CrysAlis Pro (Agilent, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur (Eos, Gemini ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44290
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis Pro; Agilent, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.688
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         10285
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+24.7380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                7429
_reflns_number_total             10285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su2644.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2238928