Iridium-Catalyzed Direct C‒H Amination with Alkylamines: Facile Oxidative Insertion of Amino Group into Iridacycle
Kim, Hyunwoo; Chang, Sukbok; ACS Catalysis 5 (2015) 6665–; doi:10.1021/acscatal.5b02165

data_4516692
_publ_section_title
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 Iridium-Catalyzed Direct C--H Amination with Alkylamines: Facile
 Oxidative Insertion of Amino Group into Iridacycle
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_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              6665
_journal_paper_doi               10.1021/acscatal.5b02165
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C124 H186 F24 Ir4 N12 O25 S8'
_chemical_formula_sum            'C124 H186 F24 Ir4 N12 O25 S8'
_chemical_formula_weight         3726.13
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 96.8149(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   11.1326(5)
_cell_length_b                   28.0168(14)
_cell_length_c                   13.6059(6)
_cell_measurement_reflns_used    176249
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.83
_cell_measurement_theta_min      2.62
_cell_volume                     4213.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            176249
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.83
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_T_max  0.5144
_exptl_absorpt_correction_T_min  0.5144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         13415
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+7.9808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                10388
_reflns_number_total             13415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5b02165_si_002.cif
_cod_data_source_block           n0343b-3
_cod_depositor_comments
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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.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4516692