Asymmetric Catalysis with an Inert Chiral-at-Metal Iridium Complex
Liang-An Chen; Weici Xu; Biao Huang; Jiajia Ma; Lun Wang; Jianwei Xi; Klaus Harms; Lei Gong; Eric Meggers; Journal of the American Chemical Society 135 (2013) 10598–10601; doi:10.1021/ja403777k

data_4120144
_publ_section_title
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 Asymmetric Catalysis with an Inert Chiral-at-Metal Iridium Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10598
_journal_page_last               10601
_journal_paper_doi               10.1021/ja403777k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C50 H34 F3 Ir N6 O5, 3(C H2 Cl2)'
_chemical_formula_sum            'C53 H40 Cl6 F3 Ir N6 O5'
_chemical_formula_weight         1302.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-11
_audit_creation_method
; 
  Olex2 1.2 
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3166(2)
_cell_length_b                   23.0618(6)
_cell_length_c                   23.8529(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5125.0(2)
_computing_cell_refinement       'Crysalis (Agilent Technologies)'
_computing_data_collection       'Crysalis (Agilent Technologies)'
_computing_data_reduction        'Crysalis (Agilent Technologies)'
_computing_molecular_graphics
; 
DIAMOND (Crystal Impact)
;
_computing_publication_material
; 
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, 
OLEX2: a complete structure solution, refinement and analysis program. 
J. Appl. Cryst. (2009). 42, 339-341. 
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Aglent Technonogies SuperNova'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24412
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.369
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
; 
 Flack x determined using 4110 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.018(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+7.2726P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9613
_reflns_number_total             10070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403777k_si_002.cif
_cod_data_source_block           L-Ir6-H
_cod_database_code               4120144
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2.a Secondary CH2 refined with riding coordinates: 
 C37(H37A,H37B), C67(H67A,H67B), C3S(H3SA,H3SB), C2S(H2SA,H2SB), C1S(H1SA,H1SB) 
2.b Aromatic/amide H refined with riding coordinates: 
 C11(H11), C12(H12), C13(H13), C14(H14), C22(H22), C32(H32), C34(H34), 
C35(H35), C42(H42), C43(H43), C44(H44), C52(H52), C53(H53), C54(H54), C55(H55), 
 C56(H56), C62(H62), C64(H64), C65(H65), C72(H72), C73(H73), C74(H74), 
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86) 
;
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.560
_shelx_res_checksum              29779
_shelxl_version_number           2013-2