A cis-IrL(CO) Group Responds to Increasing Steric Bulk of L by M-L Stretching, Not M-C-O Tilting or Bending
Tiffany Dubé; J. W. Faller; Robert H. Crabtree; Inorganic Chemistry 41 (2002) 5561–5565; doi:10.1021/ic020144+

data_4327526
_publ_contact_author_address
;
     Department of Chemistry, Yale University, New Haven, CT 06520-8107 USA
;
_publ_contact_author_email       ' Jack.faller@yale.edu '
_publ_contact_author_fax         ' (203)-432-6144 '
_publ_contact_author_name        ' J. W. Faller'
_publ_contact_author_phone       ' (203)-432-3954 '
_publ_section_title
;
 A cis-IrL(CO) Group Responds to Increasing Steric Bulk of L by M-L
 Stretching, Not M-C-O Tilting or Bending
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5561
_journal_page_last               5565
_journal_paper_doi               10.1021/ic020144+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C54 H47 Ir N O P2, B F4'
_chemical_formula_sum            'C54 H47 B F4 Ir N O P2'
_chemical_formula_weight         1066.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.227(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1303(2)
_cell_length_b                   15.1748(3)
_cell_length_c                   29.5914(5)
_cell_measurement_reflns_used    37797
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     4541.73(15)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo-SMN
_computing_publication_material  'teXsan for Windows v. 1.06 (MSC 1999)'
_computing_structure_refinement  'teXsan for Windows v. 1.06 (MSC 1999)'
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.06707
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            33992
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136.00
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.50
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.909
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment
;
included at calculated positions except for Ir-H which was refined
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.036
_refine_ls_wR_factor_ref         0.036
_reflns_number_gt                6181
_reflns_number_total             10788
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic0201442B_1.cif
_cod_data_source_block           '_2035_[IrBQ-tBU(CO)]BF4'
_cod_original_cell_volume        4541.7(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C54 H47 B F4 Ir N O P2 '
_cod_database_code               4327526