Influence of the Linker Length and Coordination Mode of (Di)Triazolylidene Ligands on the Structure and Catalytic Transfer Hydrogenation Activity of Iridium(III) Centers
Vivancos, Ángela; Albrecht, Martin; Organometallics 36 (2017) 1580–; doi:10.1021/acs.organomet.7b00140

data_4089271
_publ_section_title
;
 Influence of the Linker Length and Coordination Mode of
 (Di)Triazolylidene Ligands on the Structure and Catalytic Transfer
 Hydrogenation Activity of Iridium(III) Centers
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1580
_journal_paper_doi               10.1021/acs.organomet.7b00140
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C23 H37 Cl Ir N6, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C25 H39 Cl3 F3 Ir N6 O3 S'
_chemical_formula_weight         859.23
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-10T16:06:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.8320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.46540(10)
_cell_length_b                   19.84700(10)
_cell_length_c                   18.50640(10)
_cell_measurement_reflns_used    31068
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      1.675
_cell_volume                     6380.03(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0049628
_diffrn_orient_matrix_UB_12      0.002537
_diffrn_orient_matrix_UB_13      0.0362779
_diffrn_orient_matrix_UB_21      -0.0046272
_diffrn_orient_matrix_UB_22      -0.0354292
_diffrn_orient_matrix_UB_23      0.0006339
_diffrn_orient_matrix_UB_31      0.0402775
_diffrn_orient_matrix_UB_32      -0.003762
_diffrn_orient_matrix_UB_33      0.0185533
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.94
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85800
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.94
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.2
_diffrn_reflns_theta_min         1.556
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.558
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       plate
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         14772
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+7.4684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0
_reflns_number_gt                11978
_reflns_number_total             14772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3d.cif
_cod_data_source_block           16ma061c2_avu-173
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089271
_shelx_res_checksum              11760
_shelx_hkl_checksum              16249