Encapsulation of Thallium(I) by Tetranuclear Rhodium or Iridium Complexes: Synthesis and Molecular Structure of Heterobimetallic Complexes Stabilized by s2-d8 Bonding Interactions
Miguel A. Casado; Jesús J. Pérez-Torrente; José A. López; Miguel A. Ciriano; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 38 (1999) 2482–2488; doi:10.1021/ic980988m

data_4321996
_publ_contact_author
;
   Dr. Fernando J. Lahoz
   Departamento de Qu\'imica Inorg\'anica - I. C. M. A.
   Facultad de Ciencias
   Universidad de Zaragoza - C.S.I.C.
   50009 Zaragoza, Spain
;
_publ_contact_author_email       LAHOZ@POSTA.UNIZAR.ES
_publ_section_title
;
 Encapsulation of Thallium(I) by Tetranuclear Rhodium or Iridium
 Complexes: Synthesis and Molecular Structure of Heterobimetallic
 Complexes Stabilized by s2-d8 Bonding Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2482
_journal_page_last               2488
_journal_paper_doi               10.1021/ic980988m
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety
'(C42 H54 N2 Rh4 S4 Tl)+, (F6 P)-, (C H2 Cl2)'
_chemical_formula_sum            'C43 H56 Cl2 F6 N2 P Rh4 S4 Tl'
_chemical_formula_weight         1561.02
_chemical_name_systematic
;
 bis(mu!5$-2,6-pyridinedithiolate-S,N,S')-tetrakis-
 ((eta$4!-1,5-cyclo-octadiene)-rhodium(i))-thallium(i) hexafluorophosphate
 dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.160(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.650(2)
_cell_length_b                   21.262(4)
_cell_length_c                   21.090(4)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      12
_cell_volume                     5600.1(17)
_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, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17212
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.345
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 Azimuthal psi-scans of 12 reflections at 10\% intervals
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9826
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+23.4586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                6751
_reflns_number_total             9826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980988m.cif
_cod_data_source_block           compound3
_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 
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_cod_database_code               4321996