Novel Rhodium and Iridium Complexes Coordinated toC3-Symmetric Tris-NHC Ligands Based on a 1,3,5-Triphenylbenzene Core. Electronic and Catalytic Properties
Mejuto, Carmen; Guisado-Barrios, Gregorio; Peris, Eduardo; Organometallics 33 (2014) 3205–; doi:10.1021/om500547g

data_4083592
_publ_section_title
;
 Novel Rhodium and Iridium Complexes Coordinated toC3-Symmetric Tris-NHC
 Ligands Based on a 1,3,5-Triphenylbenzene Core. Electronic and Catalytic
 Properties
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3205
_journal_paper_doi               10.1021/om500547g
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C F3 O3 S, 2(C12 H11 N2)'
_chemical_formula_sum            'C25 H22 F3 N4 O3 S'
_chemical_formula_weight         515.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   34.2772(14)
_cell_length_b                   34.2772(14)
_cell_length_c                   14.1208(6)
_cell_measurement_reflns_used    4510
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.6240
_cell_measurement_theta_min      3.4110
_cell_volume                     14368.1(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.834
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0237304000
_diffrn_orient_matrix_UB_12      0.0206121000
_diffrn_orient_matrix_UB_13      0.0947059000
_diffrn_orient_matrix_UB_21      -0.0127744000
_diffrn_orient_matrix_UB_22      0.0370409000
_diffrn_orient_matrix_UB_23      -0.0093379000
_diffrn_orient_matrix_UB_31      -0.0443173000
_diffrn_orient_matrix_UB_32      -0.0299738000
_diffrn_orient_matrix_UB_33      0.0532844000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.834
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13623
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         60.995
_diffrn_reflns_theta_min         3.466
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description
;
;
_exptl_crystal_F_000             4806
_exptl_crystal_size_max          0.4043
_exptl_crystal_size_mid          0.1787
_exptl_crystal_size_min          0.1169
_platon_squeeze_details
;
;
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1663P)^2^+3.4246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2461
_refine_ls_wR_factor_ref         0.2626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3348
_reflns_number_total             4812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500547g_si_001.cif
_cod_data_source_block           str1616
_cod_depositor_comments
'Adding full bibliography for 4083592--4083593.cif.'
_cod_original_cell_volume        14368.1(13)
_cod_database_code               4083592
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C75 H60 N12 Ag3 F9 S3 O7'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H24(0.062) H21(0.07) H19(0.076) H22(0.081) H18(0.087) H14(0.12)
 H13(0.12) H12(0.12) H7(0.115) H6(0.122) H9(0.126) H1(0.144) H15(0.146)
 H16A(0.228) H16B(0.228) H16C(0.228) H4A(0.238) H4B(0.238) H4C(0.238) H2(0.175)
 H10(0.134)
 Fixed X: H24(0.3193) H21(0.3786) H19(0.4502) H22(0.4373) H18(0.5083)
 H14(0.57) H13(0.4836) H12(0.302) H7(0.3527) H6(0.3998) H9(0.4418) H1(0.4345)
 H15(0.5597) H16A(0.6395) H16B(0.6446) H16C(0.6422) H4A(0.5253) H4B(0.5032)
 H4C(0.4727) H2(0.568) H10(0.4879)
 Fixed Y: H24(0.5931) H21(0.5934) H19(0.7028) H22(0.5786) H18(0.6874)
 H14(0.6829) H13(0.5518) H12(0.5892) H7(0.5729) H6(0.5417) H9(0.6773)
 H1(0.5045) H15(0.5638) H16A(0.6583) H16B(0.683) H16C(0.6361) H4A(0.4795)
 H4B(0.4772) H4C(0.4549) H2(0.571) H10(0.6462)
 Fixed Z: H24(0.544) H21(0.6232) H19(0.4633) H22(0.6208) H18(0.4578)
 H14(0.5438) H13(0.53) H12(0.2916) H7(0.3654) H6(0.3622) H9(0.2115) H1(0.2602)
 H15(0.5335) H16A(0.611) H16B(0.5144) H16C(0.516) H4A(0.2725) H4B(0.1739)
 H4C(0.263) H2(0.2762) H10(0.2064)
;