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_4321825
_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         'C24 H28 I3 N4 O2 P2 Rh2 +1, I5 -1'
_chemical_formula_structural
'[Rh2 (\m2-C3 H3 N2)(\m-I)2 (C8 H11 P)2 (C O)2 I2] I5'
_chemical_formula_sum            'C24 H28 I8 N4 O2 P2 Rh2'
_chemical_formula_weight         1687.46
_chemical_name_systematic
;  (mu!2$-iodo)-bis(mu!2$-pyrazolate-N,N')-bis(carbonyl-iodo-dimethyl
  phenylphosphine-rhodium(iii)) pentaiodide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8522(5)
_cell_length_b                   13.4689(6)
_cell_length_c                   25.3911(11)
_cell_measurement_reflns_used    18743
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      1.71
_cell_volume                     4053.3(3)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25135
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.014
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.655
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.217
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       0.00043(5)
_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   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         9258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0487P)^2^+9.2941P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                8336
_reflns_number_total             9258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980650s_3.cif
_cod_data_source_block           compd18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0487P)^2^+9.2941P] 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^)+(0.0487P)^2^+9.2941P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321825