C‒H Bond Cleavage of Acetonitrile by Iridium Complexes Bearing PNP-Pincer-Type Phosphaalkene Ligands
Chang, Yung-Hung; Takeuchi, Katsuhiko; Wakioka, Masayuki; Ozawa, Fumiyuki; Organometallics 34 (2015) 1957–; doi:10.1021/acs.organomet.5b00207

data_4085860
_publ_section_title
;
 C--H Bond Cleavage of Acetonitrile by Iridium Complexes Bearing
 PNP-Pincer-Type Phosphaalkene Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1957
_journal_paper_doi               10.1021/acs.organomet.5b00207
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C51 H75 Ir K N3 O P2'
_chemical_formula_weight         1039.38
_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                90.000(8)
_cell_angle_beta                 96.747(9)
_cell_angle_gamma                90.000(8)
_cell_formula_units_Z            4
_cell_length_a                   15.021(13)
_cell_length_b                   16.507(15)
_cell_length_c                   20.16(2)
_cell_measurement_reflns_used    13521
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.2250
_cell_measurement_theta_min      2.3090
_cell_volume                     4964(8)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32089
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.9427
_exptl_absorpt_correction_T_min  0.8997
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.584
_refine_diff_density_min         -1.792
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8244
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+63.8807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2200
_reflns_number_gt                5931
_reflns_number_total             8244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00207_si_002.cif
_cod_data_source_block           complex_5
_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/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085859--4085860.cif.
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4085860