Hydrogen Activation by an Iridium(III) Complex Bearing a Bidentate Protic NH,NR-NHC∧Phosphine Ligand
Cepa, Steffen; Schulte to Brinke, Christian; Roelfes, Florian; Hahn, F. Ekkehardt; Organometallics 34 (2015) 5454–; doi:10.1021/acs.organomet.5b00799

data_4088005
_publ_section_title
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 Hydrogen Activation by an Iridium(III) Complex Bearing a Bidentate Protic
 NH,NR-NHC&#x2227;Phosphine Ligand
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_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5454
_journal_paper_doi               10.1021/acs.organomet.5b00799
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C33 H51 Ir N2 P, B F4'
_chemical_formula_sum            'C33 H51 B F4 Ir N2 P'
_chemical_formula_weight         785.78
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 115.7590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8788(8)
_cell_length_b                   13.5847(5)
_cell_length_c                   12.4615(5)
_cell_measurement_reflns_used    23373
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.009
_cell_measurement_theta_min      2.2315
_cell_volume                     3335.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29615
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         31.05
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    4.098
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         10449
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.4046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                10303
_reflns_number_total             10449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00799_si_002.cif
_cod_data_source_block           '[5]BF4'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088005