Synthesis of the homoleptic rhodium(III) complex [Rh(C6Cl5)3]. Molecular structures of [Rh(C6Cl5)3] and [Rh(C6Cl4‒C6Cl4)(C6Cl5)(SC4H8)2]
García, María P.; Jiménez, M. Victoria; Lahoz, Fernando J.; López, José A.; Oro, Luis A.; Journal of the Chemical Society, Dalton Transactions  (1998) 4211–; doi:10.1039/a806538a

data_7027081
_publ_section_title
;
 Synthesis of the homoleptic rhodium(III) complex [Rh(C6Cl5)3]. Molecular
 structures of [Rh(C6Cl5)3] and [Rh(C6Cl4--C6Cl4)(C6Cl5)(SC4H8)2]
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4211
_journal_paper_doi               10.1039/a806538a
_journal_year                    1998
_chemical_formula_moiety         'C26 H16 Cl13 Rh S2'
_chemical_formula_sum            'C26 H16 Cl13 Rh S2'
_chemical_formula_weight         956.27
_chemical_name_systematic
;
 (octachloro-2,2'-biphenylene)-(pentachlorophenyl)-
 bis(tetrahidrothiophene)-rhodium(III)
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.805(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2192(5)
_cell_length_b                   32.660(2)
_cell_length_c                   11.3747(7)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     3295.4(4)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'XP, SHELXTL v.5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6264
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.5625
_exptl_absorpt_correction_T_min  0.5147
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details
;
 Azimuthal psi-scans of 12 reflections at 10\% intervals.
 Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5795
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+4.3269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                4613
_reflns_number_total             5795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            806538Asup1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3295.4(3)
_cod_database_code               7027081