Catalyst Activation by Loss of Cyclopentadienyl Ligands in Hydrogen Transfer Catalysis with Cp*IrIIIComplexes
Campos, Jesús; Hintermair, Ulrich; Brewster, Timothy P.; Takase, Michael K.; Crabtree, Robert H.; ACS Catalysis 4 (2014) 973–; doi:10.1021/cs401138f

data_4510031
_publ_contact_author
;
 Dr. Robert H. Crabtree           
 The Department of Chemistry 
 Yale University 
 P. O. Box 208107 
 New Haven 
 Connecticut 06520 USA.
;
_publ_section_title
;
 Catalyst Activation by Loss of Cyclopentadienyl Ligands in Hydrogen
 Transfer Catalysis with Cp*IrIIIComplexes
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              973
_journal_paper_doi               10.1021/cs401138f
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C36 H63 B Cl F4 Ir N4 O'
_chemical_formula_weight         882.36
_chemical_name_systematic
; 
 ? 
;
_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                 112.440(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9451(10)
_cell_length_b                   22.7483(4)
_cell_length_c                   13.5566(3)
_cell_measurement_reflns_used    150178
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      3.0
_cell_volume                     3974.9(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12 (Rigaku)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 (Rigaku)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12 (Rigaku)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_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  0.1094
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            219215
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  0.7224
_exptl_absorpt_correction_T_min  0.5431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+9.0118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                7777
_reflns_number_total             9120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs401138f_si_007.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3974.9(3)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4510031