Tris(η^5^-cyclopentadienyl)-tris[η^6^-[9,10-dihydroanthracene-9,10-<i>endo</i>-3',4'-(<i>N</i>-benzyl)pyrrolidine]]triruthenium(II) tris(hexafluorophosphate) acetone disolvate
Bratko, Ielyzaveta; Mallet-Ladeira, Sonia; Saffon, Nathalie; Teuma, Emmanuelle; Gómez, Montserrat; Acta Crystallographica Section E 68 (2012) m1313–m1314; doi:10.1107/S1600536812040652

data_2236642
_publ_section_title
;
 Tris(\h^5^-cyclopentadienyl)-tris[\h^6^-[9,10-dihydroanthracene-9,10-<i>endo</i>-3',4'-(<i>N</i>-benzyl)pyrrolidine]]triruthenium(II)
 tris(hexafluorophosphate) acetone disolvate
;
_journal_coeditor_code           SU2499
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1313
_journal_page_last               m1314
_journal_paper_doi               10.1107/S1600536812040652
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Ru3 (C25 H23 N) (C5 H5)3] , 3P F6 , 2C3 H6 O]'
_chemical_formula_moiety         'C40 H38 N Ru3, 3(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C46 H50 F18 N O2 P3 Ru3'
_chemical_formula_weight         1386.99
_chemical_name_common
;
Tris(\h^5^-cyclopentadienyl)-[(tris-\h^6^)-(9,10-dihydroanthracene-9,10-endo-\
3',4'-(<i>N</i>-benzyl)-pyrrolidine)]-triruthenium(II)
tris(hexafluorophosphate)
;
_chemical_name_systematic
;
Tris(\h^5^-cyclopentadienyl)-tris[\h^6^-[9,10-dihydroanthracene-9,10-
<i>endo</i>-3',4'-(<i>N</i>-benzyl)pyrrolidine]]triruthenium(II)
tris(hexafluorophosphate) acteone disolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.038(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6054(7)
_cell_length_b                   36.567(2)
_cell_length_c                   14.4207(10)
_cell_measurement_reflns_used    9276
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.90
_cell_measurement_theta_min      2.46
_cell_volume                     4891.7(6)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD Quazar'
_diffrn_measurement_method       '\f and \w'
_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  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75190
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.765
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         11960
_refine_ls_number_restraints     738
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0298P)^2^+6.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                7646
_reflns_number_total             11960
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2499.cif
_cod_data_source_block           I
_cod_original_cell_volume        4891.6(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2236642
_cod_database_fobs_code          2236642