Syntheses, Structures, and Reactivity of New Pentamethylcyclopentadienyl-Rhodium(III) and -iridium(III) 4-Acyl-5-Pyrazolonate Complexes
Claudio Pettinari; Riccardo Pettinari; Mauro Fianchini; Fabio Marchetti; Brian W. Skelton; Allan H. White; Inorganic Chemistry 44 (2005) 7933–7942; doi:10.1021/ic050985r

data_4309884
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
Syntheses, Structures, and Reactivity of New
Pentamethylcyclopentadienyl-Rhodium(III) and -iridium(III)
4-Acyl-5-Pyrazolonate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7933
_journal_page_last               7942
_journal_paper_doi               10.1021/ic050985r
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C22 H26 Cl Ir N2 O2'
_chemical_formula_weight         578.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   primary
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   primary
_cell_angle_alpha                90.00000
_cell_angle_beta                 96.470(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   8.6997(6)
_cell_length_b                   17.0490(10)
_cell_length_c                   13.9360(9)
_cell_measurement_reflns_used    5964
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      .044
_cell_measurement_theta_min      .045
_cell_volume                     2053.8(2)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .045
_diffrn_reflns_av_sigmaI/netI    .08
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42837
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.651
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.87
_exptl_crystal_description       chip
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          .12
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .06
_refine_diff_density_max         2.535
_refine_diff_density_min         -1.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .984
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .064
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .045
_refine_ls_wR_factor_ref         .04
_reflns_d_resolution_high        .583
_reflns_d_resolution_low         10.726
_reflns_Friedel_coverage         0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                7799
_reflns_number_total             10806
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            ic050985rsi20050616_065955_2.cif
_cod_data_source_block           cpirqc
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_formula_sum        'C22 H26 Cl1 Ir1 N2 O2'
_cod_database_code               4309884