Bis(triphenylphosphoranylidene)ammonium docosacarbonyl(μ~8~-phosphido)octaruthenate chloroform solvate
Michael D. Randles; Anthony C. Willis; Marie P. Cifuentes; Mark G. Humphrey; Acta Crystallographica Section E 62 (2006) m2350–m2351; doi:10.1107/S1600536806034052

data_2210101
_publ_section_title
;
 Bis(triphenylphosphoranylidene)ammonium
 docosacarbonyl(\m~8~-phosphido)octaruthenate chloroform solvate
;
_journal_coeditor_code           BM2003
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2350
_journal_page_last               m2351
_journal_paper_doi               10.1107/S1600536806034052
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C36 H30 N1 P2) [Ru8 P (C O)22], C H Cl3'
_chemical_formula_moiety         'C36 H30 N1 P2 +, C22 O22 P Ru8 -, C H Cl3'
_chemical_formula_sum            'C59 H31 Cl3 N O22 P3 Ru8'
_chemical_formula_weight         2113.73
_chemical_name_systematic
;
Bis(triphenylphosphoranylidene)ammonium
docosacarbonyl(\m~8~-phosphido)octaruthenate chloroform solvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1786(2)
_cell_length_b                   10.54480(10)
_cell_length_c                   32.9569(4)
_cell_measurement_reflns_used    86582
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     6665.02(12)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_publication_material
;
CRYSTALS
;
_computing_structure_refinement
;
CRYSTALS (Betteridge et al., 2003)
;
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            78313
_diffrn_reflns_theta_full        27.483
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.677
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_description       plate
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.01
_refine_diff_density_min         -1.26
_refine_ls_abs_structure_details
'Flack (1983); 7252 Friedel-pairs, partially inversion twinned'
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         10343
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.04
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;w =
 [1-(F~o~-F~c~)^2^/36\s^2^(F)]^2^/[0.282T~o~(x)-0.0449T~1~(x)+0.108T~2~(x)]
where
 T~i~ are the Chebychev polynomials and x=F~c~/F~max~
(Prince, 1982; Watkin,
 1994)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0362
_refine_ls_wR_factor_gt          0.0233
_refine_ls_wR_factor_ref         0.0233
_reflns_number_gt                10343
_reflns_number_total             15035
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bm2003.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C59 H31 Cl3 N1 O22 P3 Ru8'
_cod_database_code               2210101
_cod_database_fobs_code          2210101