Vibrational circular dichroism and single crystal X-Ray diffraction analyses of [Ir(bzq)2(phen)](+) (bzq = benzo[h]quinoline; phen = 1,10-phenanthroline): absolute configuration and role of CH-π interaction in molecular packing.
Takimoto, Kazuyoshi; Watanabe, Yutaka; Mori, Shigeki; Sato, Hisako; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4397–4402; doi:10.1039/c7dt00606c

data_7042318
_publ_section_title
;
 Vibrational circular dichroism and single crystal X-Ray diffraction
 analyses of [Ir(bzq)2(phen)](+) (bzq = benzo[h]quinoline; phen =
 1,10-phenanthroline): absolute configuration and role of CH-\p
 interaction in molecular packing.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4397
_journal_page_last               4402
_journal_paper_doi               10.1039/c7dt00606c
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H24 Ir N4, C2 F3 O2, C H2 Cl2'
_chemical_formula_sum            'C41 H26 Cl2 F3 Ir N4 O2'
_chemical_formula_weight         926.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-01-16 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.63469(10)
_cell_length_b                   9.63469(10)
_cell_length_c                   36.5088(5)
_cell_measurement_reflns_used    38143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.12
_cell_volume                     3389.01(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            48848
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    4.160
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 3612 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     460
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0207P)^2^+3.0730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7754
_reflns_number_total             8185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00606c2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7042317--7042318.cif.'
_cod_original_cell_volume        3389.01(8)
_cod_database_code               7042318
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              17745