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_4089275
_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_absolute_configuration rmad
_chemical_formula_sum            'C21 H32 Cl2 F3 Ir N6 O3 S'
_chemical_formula_weight         768.68
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-10T14:58:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.3700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6608(2)
_cell_length_b                   8.63570(10)
_cell_length_c                   13.65320(10)
_cell_measurement_reflns_used    12242
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.952
_cell_measurement_theta_min      1.929
_cell_volume                     1432.26(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
        (compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
        (compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
        (compiled Dec  9 2014,15:38:47)
;
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(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 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0190302
_diffrn_orient_matrix_UB_12      -0.0448567
_diffrn_orient_matrix_UB_13      -0.0450578
_diffrn_orient_matrix_UB_21      -0.0461117
_diffrn_orient_matrix_UB_22      -0.023974
_diffrn_orient_matrix_UB_23      0.0159798
_diffrn_orient_matrix_UB_31      -0.0303403
_diffrn_orient_matrix_UB_32      0.0645425
_diffrn_orient_matrix_UB_33      -0.0253723
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23112
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.554
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.974
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
        (compiled Dec  9 2014,15:38:47)
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            'translucent light yellow'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.2269
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.0461
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2480 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.021
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.3685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.87
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     1
_reflns_number_gt                5568
_reflns_number_total             5851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4a.cif
_cod_data_source_block           16ma067
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4089275
_shelx_res_checksum              1712
_shelx_hkl_checksum              86724