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_4080963
_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_formula_moiety         'C23 H30 Cl N2 Pd'
_chemical_formula_sum            'C23 H30 Cl N2 Pd'
_chemical_formula_weight         476.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.016(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5718(2)
_cell_length_b                   10.47820(10)
_cell_length_c                   15.3990(10)
_cell_measurement_reflns_used    12852
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      69.20
_cell_measurement_theta_min      7.30
_cell_volume                     2259.95(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 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    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     1.54187
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13567
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         7.30
_exptl_absorpt_coefficient_mu    7.765
_exptl_absorpt_correction_T_max  0.3057
_exptl_absorpt_correction_T_min  0.3057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4074
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                3469
_reflns_number_total             4074
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4002928_si_002.cif
_cod_data_source_block           a3
_cod_original_cell_volume        2259.95(15)
_cod_database_code               4080963