Enantioselective Excited-State Photoreactions Controlled by a Chiral Hydrogen-Bonding Iridium Sensitizer.
Skubi, Kazimer L.; Kidd, Jesse B.; Jung, Hoimin; Guzei, Ilia A.; Baik, Mu-Hyun; Yoon, Tehshik P.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10586

data_4126742
_publ_section_title
;
 Enantioselective Excited-State Photoreactions Controlled by a Chiral
 Hydrogen-Bonding Iridium Sensitizer.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10586
_journal_year                    2017
_chemical_formula_sum            'C65.69 H32.07 B F36 Ir N5 O0.84'
_chemical_formula_weight         1791.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.606(7)
_cell_length_b                   18.804(8)
_cell_length_c                   19.121(7)
_cell_measurement_reflns_used    9202
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.39
_cell_volume                     6689(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            131360
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.118
_diffrn_reflns_theta_min         1.515
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  .43
_exptl_absorpt_correction_T_min  .39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       plate
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
; 
 Flack x determined using 12207 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.0247(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1780
_refine_ls_number_reflns         29402
_refine_ls_number_restraints     4716
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+12.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                27172
_reflns_number_total             29402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6b.cif
_cod_data_source_block           yoon51
_cod_database_code               4126742
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              59868
_shelx_hkl_checksum              53378