Indazolin-s-ylidene‒N-Heterocyclic Carbene Complexes of Rhodium, Palladium, and Gold: Synthesis, Characterization, and Catalytic Hydration of Alkynes
Zhou, Yang; Liu, Qingjie; Lv, Weifeng; Pang, Qingyu; Ben, Rong; Qian, Yong; Zhao, Jing; Organometallics 32 (2013) 3753–; doi:10.1021/om4002928

data_4080962
_publ_section_title
;
 Indazolin-s-ylidene--N-Heterocyclic Carbene Complexes of Rhodium,
 Palladium, and Gold: Synthesis, Characterization, and Catalytic Hydration
 of Alkynes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3753
_journal_paper_doi               10.1021/om4002928
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H35 Cl N2 Rh'
_chemical_formula_weight         537.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   10.9071(2)
_cell_length_b                   22.1098(4)
_cell_length_c                   32.683(2)
_cell_measurement_reflns_used    51492
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      6.60
_cell_volume                     7881.6(5)
_computing_cell_refinement       'CrystalClear-SM Auto 2.0 r4'
_computing_data_collection       'CrystalClear-SM Auto 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Auto 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1197
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            91422
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         6.59
_exptl_absorpt_coefficient_mu    6.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.292
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881.  6386 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.025(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         14305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.959
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2137
_refine_ls_wR_factor_ref         0.2484
_reflns_number_gt                8922
_reflns_number_total             14305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002928_si_002.cif
_cod_data_source_block           wa10
_cod_original_cell_volume        7881.7(6)
_cod_database_code               4080962