C−H Oxidative Addition to a (PNP)Ir Center and Ligand-Induced Reversal of Benzyl/Aryl Selectivity
Zhu, Yanjun; Fan, Lei; Chen, Chun-Hsing; Finnell, Shannon R.; Foxman, Bruce M.; Ozerov, Oleg V.; Organometallics 26 (2007) 6701–; doi:10.1021/om701110y

data_4074106
_publ_section_title
;
 C&#x2212;H Oxidative Addition to a (PNP)Ir Center and Ligand-Induced
 Reversal of Benzyl/Aryl Selectivity
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6701
_journal_paper_doi               10.1021/om701110y
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C38 H55.00 Ir1 N2 P2 S1'
_chemical_formula_sum            'C38 H55 Ir N2 P2 S'
_chemical_formula_weight         826.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-07-07
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 94.126(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7373(9)
_cell_length_b                   17.2111(13)
_cell_length_c                   18.3398(13)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3695.3(5)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'KappaCCD ApexII'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            113849
_diffrn_reflns_theta_full        29.504
_diffrn_reflns_theta_max         30.106
_diffrn_reflns_theta_min         1.625
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.785
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680.001
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.67
_refine_diff_density_min         -1.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10804
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.007390
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 21.6 30.7 14.5 4.38 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0591
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0591
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8478
_reflns_number_total             10804
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0305
_oxford_refine_ls_scale          0.22048(5)
_oxford_reflns_number_all        10804
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ103_0m in P2(1)/n'
_cod_data_source_file            om701110y-file001.cif
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C38 H55.00 Ir1 N2 P2 S1'
_cod_database_code               4074106