Synthesis and Molecular Structure of [{(HBpz3)Rh(PPh3)(μ-Cl)2}2Ag]BF4 (Hpz = Pyrazole), a Heterotrinuclear Rh2Ag Compound with Square-Planar Silver(I)
Daniel Carmona; Fernando Viguri; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 41 (2002) 2385–2388; doi:10.1021/ic011217c

data_4317948
_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
;
 Synthesis and Molecular Structure of [{(HBpz3)Rh(PPh3)(\m-Cl)2}2Ag]BF4
 (Hpz = Pyrazole), a Heterotrinuclear Rh2Ag Compound with Square-Planar
 Silver(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2385
_journal_page_last               2388
_journal_paper_doi               10.1021/ic011217c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C54 H50 Ag B2 Cl4 N12 P2 Rh2 1+, B F4 1-'
_chemical_formula_sum            'C54 H50 Ag B3 Cl4 F4 N12 P2 Rh2'
_chemical_formula_weight         1492.92
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.262(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.329(4)
_cell_length_b                   10.3786(15)
_cell_length_c                   23.883(4)
_cell_measurement_reflns_used    57
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      18.3
_cell_measurement_theta_min      10
_cell_volume                     6029.0(17)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTL v6.10, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens-Stoe AED-2 diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10598
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.7319
_exptl_absorpt_correction_T_min  0.6671
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;

  Azimuthal psi-scans of 10 reflections at 10\% intervals.

  Data corrected with the program EMPIR (Stoe)

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5329
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                3260
_reflns_number_total             5329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011217c.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        6029.1(16)
_cod_database_code               4317948