Tetranuclear [Rh4(μ-PyS2)2(diolefin)4] Complexes as Building Blocks for New Inorganic Architectures: Synthesis of Coordination Polymers and Heteropolynuclear Complexes with Electrophilic d8 and d10 Metal Fragments
Miguel A. Casado; Jesús J. Pérez-Torrente; Miguel A. Ciriano; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 43 (2004) 1558–1567; doi:10.1021/ic034893i

data_4310603
_publ_contact_author_address
;
  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_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
 Tetranuclear [Rh4(\m-PyS2)2(diolefin)4] Complexes as Building Blocks for
 New Inorganic Architectures: Synthesis of Coordination Polymers and
 Heteropolynuclear Complexes with Electrophilic d8 and d10 Metal Fragments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1558
_journal_page_last               1567
_journal_paper_doi               10.1021/ic034893i
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
; C94 H60 Au2 F16 N2 P2 Rh4 S4, 2(Cl O4), 2(C H2 Cl2), C3 H6 O,
  4(C6 H14)
;
_chemical_formula_sum            'C123 H126 Au2 Cl6 F16 N2 O9 P2 Rh4 S4'
_chemical_formula_weight         3288.71
_chemical_name_systematic
; 
 ? 
;
_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                 115.2690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.7939(12)
_cell_length_b                   21.9335(11)
_cell_length_c                   24.5094(12)
_cell_measurement_reflns_used    5264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      2.46
_cell_volume                     11081.0(10)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.2019
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59718
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             6512
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1271
_refine_ls_number_reflns         19583
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                10069
_reflns_number_total             19583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034893isi20030729_034816.cif
_cod_data_source_block           mac36az
_cod_database_code               4310603