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_4321823
_publ_contact_author
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   Fernando J. Lahoz
   Departamento de Qu\'imica Inorg\'anica
   Facultad de Ciencias
   Universidad de Zaragoza - C.S.I.C.
   50009 Zaragoza, Spain
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_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         'C14 H24 I2 N4 O8 P2 Rh2'
_chemical_formula_structural     '[Rh (C3 H3 N2) (C O) I (P (C H3 O)3)]2'
_chemical_formula_sum            'C14 H24 I2 N4 O8 P2 Rh2'
_chemical_formula_weight         897.93
_chemical_name_systematic
' bis-(mu!2$-pyrazolate-N,N')-carbonyl-iodo-trimethylphosphite-rhodium(ii))'
_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                83.94(3)
_cell_angle_beta                 79.975(15)
_cell_angle_gamma                83.97(3)
_cell_formula_units_Z            4
_cell_length_a                   10.550(2)
_cell_length_b                   15.763(3)
_cell_length_c                   16.353(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      9
_cell_volume                     2652.6(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER AXS-Stoe diffractometer'
_diffrn_measurement_method       '\w/\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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9365
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    3.736
_exptl_absorpt_correction_T_max  0.212
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0589P)^2^+1.9609P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                6594
_reflns_number_total             9336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980650s_1.cif
_cod_data_source_block           compd7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0589P)^2^+1.9609P] 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^)+(0.0589P)^2^+1.9609P] 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_cell_volume        2652.5(9)
_cod_database_code               4321823