Key Factors Determining the Course of Methyl Iodide Oxidative Addition to Diamidonaphthalene-Bridged Diiridium(I) and Dirhodium(I) Complexes
M. Victoria Jiménez; Eduardo Sola; M. Angeles Egea; Aline Huet; Ana C. Francisco; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 39 (2000) 4868–4878; doi:10.1021/ic000497d

data_4321473
_publ_contact_author
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica
  Facultad de Ciencias
  Universidad de Zaragoza
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@posta.unizar.es
_publ_section_title
;
 Key Factors Determining the Course of Methyl Iodide Oxidative Addition to
 Diamidonaphthalene-Bridged Diiridium(I) and Dirhodium(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4868
_journal_page_last               4878
_journal_paper_doi               10.1021/ic000497d
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C31 H53 I N2 O2 P2 Rh2'
_chemical_formula_sum            'C31 H53 I N2 O2 P2 Rh2'
_chemical_formula_weight         880.41
_chemical_name_systematic
; acetyl iodide carbonyl triisopropylphosphine di-mu-diamidonaphthalene
  di-rhodium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.449(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7147(9)
_cell_length_b                   11.8158(8)
_cell_length_c                   21.6449(16)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     3609.3(4)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP program, SHELXTL v. 5.0 (Bruker, 1994)'
_computing_publication_material  'CIFTAB program (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  Siemens-P4
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'norma-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7153
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  0.7276
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; The method for absorption correction was based on the observed morphology
 of the crystal; faces and distances to a common point are as follows: 1 1 0,
 0.110 mm; -1 -1 0, 0.200 mm; -1 1 0, 0.150 mm; 1 -1 0, 0.170 mm; 1 0 -2,
 0.090; -1 0 2, 0.090 mm). The correction was performed using the XPREP
 program of the SHELXTL package (Bruker, 1994)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic blocks'
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         6350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+5.3591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                5405
_reflns_number_total             6350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000497d_1.cif
_cod_data_source_block           compound12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+5.3591P] where P=(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=1/[\s^2^(Fo^2^)+(0.0303P)^2^+5.3591P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321473