Tri-μ-chlorido-bis[(η^5^-pentamethylcyclopentadienyl)rhodium(III)] hexafluoridophosphate from synchrotron radiation
Ezzedinloo, Lida; Shrestha, Sumi; Bhadbhade, Mohan; Colbran, Stephen; Acta Crystallographica Section E 70 (2014) m14–m15; doi:10.1107/S1600536813032480

data_2239109
_publ_section_title
;
 Tri-\m-chlorido-bis[(\h^5^-pentamethylcyclopentadienyl)rhodium(III)]
 hexafluoridophosphate from synchrotron radiation
;
_journal_coeditor_code           TK5276
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m14
_journal_page_last               m15
_journal_paper_doi               10.1107/S1600536813032480
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Rh2 (C10 H15)2 Cl3] P F6'
_chemical_formula_moiety         'C20 H30 Cl3 Rh2 +, F6 P -'
_chemical_formula_sum            'C20 H30 Cl3 F6 P Rh2'
_chemical_formula_weight         727.58
_chemical_name_common            '[Cp*RuCl3RuCp*][PF6]'
_chemical_name_systematic
;
Tri-\m-chlorido-bis[(\h^5^-pentamethylcyclopentadienyl)rhodium(III)]
hexafluoridophosphate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                64.28(3)
_cell_angle_beta                 82.42(3)
_cell_angle_gamma                86.70(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0970(16)
_cell_length_b                   12.604(3)
_cell_length_c                   14.441(3)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     1316.2(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips <i>et al.</i>, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and OLEX-2 (Dolomanov <i>et al.</i>,
2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.807
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.669
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.565
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+3.0381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                4064
_reflns_number_total             4158
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5276sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1316.1(6)
_cod_database_code               2239109
_cod_database_fobs_code          2239109
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              17045
_shelx_res_checksum              99262
_shelxl_version_number           2.013