Water Attack Umpolung Aromatic Systems To Release Hydrogen
Tsun-Ren Chen; Hsiu-Pen Lee; Jhy-Der Chen; Inorganic Chemistry 50 (2011) 3645–3650; doi:10.1021/ic1025944

data_4324892
_publ_section_title
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 Water Attack Umpolung Aromatic Systems To Release Hydrogen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3645
_journal_page_last               3650
_journal_paper_doi               10.1021/ic1025944
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C44 H27 Cl F4 Ir N2 O2 P, C H2 Cl2 '
_chemical_formula_sum            'C45 H29 Cl3 F4 Ir N2 O2 P'
_chemical_formula_weight         1035.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.340(2)
_cell_angle_beta                 70.900(2)
_cell_angle_gamma                77.471(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5124(2)
_cell_length_b                   13.2493(4)
_cell_length_c                   15.7584(4)
_cell_measurement_reflns_used    18459
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      29.1809
_cell_measurement_theta_min      2.7330
_cell_volume                     2020.43(9)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_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      105(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17548
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.13
_refine_diff_density_max         6.561
_refine_diff_density_min         -3.543
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         9336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+39.8496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                7474
_reflns_number_total             9336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1025944_si_002_1.cif
_cod_data_source_block           2a
_cod_database_code               4324892