Intra- and Intermolecular C‒H Activation by Bis(phenolate)pyridineiridium(III) Complexes
Fu, Ross; Bercaw, John E.; Labinger, Jay A.; Organometallics 30 (2011) 6751–; doi:10.1021/om201069k

data_4083323
_publ_section_title
;
 Intra- and Intermolecular C--H Activation by
 Bis(phenolate)pyridineiridium(III) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6751
_journal_paper_doi               10.1021/om201069k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C73 H82 Ir N O2 P2, C5 H12'
_chemical_formula_sum            'C78 H94 Ir N O2 P2'
_chemical_formula_weight         1331.68
_chemical_name_systematic
;

 ?

;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.373(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8289(8)
_cell_length_b                   23.8694(10)
_cell_length_c                   17.4749(8)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.83
_cell_measurement_theta_min      2.39
_cell_volume                     6856.6(5)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 14 settings'
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            184039
_diffrn_reflns_theta_full        33.55
_diffrn_reflns_theta_max         33.55
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.907
_refine_diff_density_min         -2.314
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.140
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         24527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.140
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                19762
_reflns_number_total             24527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            11-Ir(PPh3)2H-ruf12.cif
_cod_data_source_block           ruf12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        6856.5(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4083323