Oxidative-Addition Reactions of Diiodine to Dinuclear Rhodium Pyrazolate Complexes
Cristina Tejel; Marta Bordonaba; Miguel A. Ciriano; Andrew J. Edwards; William Clegg; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 38 (1999) 1108–1117; doi:10.1021/ic980650s

data_4321824
_publ_contact_author
;
   Fernando J. Lahoz
   Departamento de Qu\'imica Inorg\'anica
   Facultad de Ciencias
   Universidad de Zaragoza - C.S.I.C.
   50009 Zaragoza, Spain
;
_publ_contact_author_email       LAHOZ@POSTA.UNIZAR.ES
_publ_section_title
;
 Oxidative-Addition Reactions of Diiodine to Dinuclear Rhodium Pyrazolate
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1108
_journal_page_last               1117
_journal_paper_doi               10.1021/ic980650s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C50 H48 I2 N4 O2 P2 Rh2, 0.5(C4 H10 O)'
_chemical_formula_structural
'[Rh2 (\m2-C3 H3 N2) (\m2-C O) (C21 H21 P)2 I2 (CO)]'
_chemical_formula_sum            'C52 H53 I2 N4 O2.5 P2 Rh2'
_chemical_formula_weight         1295.54
_chemical_name_systematic
;  
(mu!2$-pyrazolate-N,N')-(mu!2$-carbonyl)-(carbonyl-iodo-tritolylphosphine
 rhodium(iii))-(iodo-tritolylphosphine-rhodium(iii)) diethylether solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.340(2)
_cell_angle_beta                 96.410(2)
_cell_angle_gamma                110.191(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3869(9)
_cell_length_b                   16.2642(13)
_cell_length_c                   16.5072(14)
_cell_measurement_reflns_used    11823
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      1.91
_cell_volume                     2822.8(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'SHELXTL v. 5 (Siemens, 1994)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'BRUKER AXS-SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19571
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00020(11)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         12242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.155
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                8412
_reflns_number_total             12242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980650s_2.cif
_cod_data_source_block           compd10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=3D1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C52 H53 I2 N4 O2.50 P2 Rh2'
_cod_database_code               4321824