Preparation of single enantiomers of chiral at metal bis-cyclometallated iridium complexes
David L. Davies; Kuldip Singh; Shalini Singh; Barbara Villa-Marcos; Chem.Commun. 49 (2013) 6546–; doi:10.1039/c3cc43121e

data_7109498
_publ_section_title
;
 Preparation of single enantiomers of chiral at metal bis-cyclometallated
 iridium complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6546
_journal_paper_doi               10.1039/c3cc43121e
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ,rm
_chemical_formula_moiety         'C33 H28 Ir N5 O, C H3 OH'
_chemical_formula_sum            'C34 H32 Ir N5 O2'
_chemical_formula_weight         734.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.794(4)
_cell_length_b                   11.361(5)
_cell_length_c                   29.429(12)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.142
_cell_measurement_theta_min      2.265
_cell_volume                     2940(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1160
_diffrn_reflns_av_sigmaI/netI    0.1155
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            23226
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    4.582
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 7138 reflections(SADABS);Rint 0.1889 before
correction and 0.0701 after.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                4827
_reflns_number_total             5780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43121e.txt
_cod_data_source_block           09081
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7109498