Catalytic Coupling between Unactivated Aliphatic C-H Bonds and Alkynes via a Metal-Hydride Pathway.
Xu, Yan; Young, Michael C.; Dong, Guangbin; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b02020

data_4125914
_publ_section_title
;
 Catalytic Coupling between Unactivated Aliphatic C-H Bonds and Alkynes
 via a Metal-Hydride Pathway.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b02020
_journal_year                    2017
_chemical_formula_moiety         'C19 H31 Cl Ir N3'
_chemical_formula_sum            'C19 H31 Cl Ir N3'
_chemical_formula_weight         529.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 98.032(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.242(6)
_cell_length_b                   11.996(6)
_cell_length_c                   12.795(6)
_cell_measurement_reflns_used    3896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0117
_cell_measurement_theta_min      1.5534
_cell_volume                     2012.6(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.301
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    6.772
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1040
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_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.102
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     228
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+3.1012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3846
_reflns_number_total             4605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02020_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4973 2017-02-22 13:04:09Z antanas 

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         264.56
_cod_original_formula_moiety         C9.50H15.50Cl0.50Ir0.50N1.50
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'C9.50 H15.50 Cl0.50 Ir0.50 N1.50'
_cod_database_code               4125914
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.430
_shelx_estimated_absorpt_t_max   0.773
_shelx_res_checksum              55588
_shelx_hkl_checksum              91807