Exploring the Scope of a Novel Ligand Class: Synthesis and Catalytic Examination of Metal Complexes with 'Normal' 1,2,3-Triazolylidene Ligands
Lars-Arne Schaper; Lilian Graser; Xuhui Wei; Rui Zhong; Karl Öfele; Alexander Pöthig; Mirza Cokoja; Bettina Bechlars; Wolfgang A. Herrmann; Fritz E. Kühn; Inorganic Chemistry 52 (2013) 6142–6152; doi:10.1021/ic400533u

data_4334953
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl f\"ur Anorganische Chemie,
       Technische Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.
;
_publ_contact_author_email       alexander.poethig@tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Alexander Poethig
;
_publ_contact_author_phone       '+49(0)89 289 13133'
_publ_section_title
;
 Exploring the Scope of a Novel Ligand Class: Synthesis and Catalytic
 Examination of Metal Complexes with 'Normal' 1,2,3-Triazolylidene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6142
_journal_page_last               6152
_journal_paper_doi               10.1021/ic400533u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C29 H35 Cl N3 Rh'
_chemical_formula_sum            'C29 H35 Cl N3 Rh'
_chemical_formula_weight         563.96
_space_group_IT_number           14
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.846(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1793(3)
_cell_length_b                   19.8096(7)
_cell_length_c                   13.1890(5)
_cell_measurement_reflns_used    9106
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.3336
_cell_measurement_theta_min      2.5829
_cell_volume                     2627.90(16)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed-tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50409
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.7796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                4683
_reflns_number_total             5347
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400533u_si_004.cif
_cod_data_source_block           Compound_B2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334953