Preparation of metalated azine complexes of iridium(iii)
Albertin, Gabriele; Antoniutti, Stefano; Bortoluzzi, Marco; Castro, Jesús; Sibilla, Francesca; Trave, Enrico; New J. Chem. 41 (2017) 12976–12988; doi:10.1039/C7NJ02224G

data_7056666
_publ_section_title
;
 Preparation of metalated azine complexes of iridium(iii)
;
_journal_issue                   21
_journal_name_full               'New J. Chem.'
_journal_page_first              12976
_journal_page_last               12988
_journal_paper_doi               10.1039/C7NJ02224G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C30 H41 Ir N2 O3 P, C24 H20 B'
_chemical_formula_sum            'C54 H61 B Ir N2 O3 P'
_chemical_formula_weight         1020.02
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-22 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9894(6)
_cell_length_b                   17.6752(7)
_cell_length_c                   19.1128(8)
_cell_measurement_reflns_used    9540
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.42
_cell_volume                     4725.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_source         'Incoatec high brillance I\muS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37601
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.305
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 4858 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         11739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+1.8253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                11241
_reflns_number_total             11739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02224g3.cif
_cod_data_source_block           fq28_29_xt
_cod_database_code               7056666
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.456
_shelx_estimated_absorpt_t_max   0.613
_shelx_res_checksum              58002