Synthesis, Characterization, and X-ray Molecular Structure of Tantalum CCC-N-Heterocyclic Carbene (CCC-NHC) Pincer Complexes with Imidazole- and Triazole-Based Ligands
Helgert, Theodore R.; Hollis, T. Keith; Oliver, Allen G.; Valle, Henry U.; Wu, Yunshan; Webster, Charles Edwin; Organometallics 33 (2014) 952–; doi:10.1021/om401063e

data_4082370
_publ_section_title
;
 Synthesis, Characterization, and X-ray Molecular Structure of Tantalum
 CCC-N-Heterocyclic Carbene (CCC-NHC) Pincer Complexes with Imidazole- and
 Triazole-Based Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              952
_journal_paper_doi               10.1021/om401063e
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C25.83 H39.49 I1.08 N5.92 Ta'
_chemical_formula_sum            'C25.831 H39.493 I1.085 N5.915 Ta'
_chemical_formula_weight         751.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_primary     direct
_audit_creation_date             2013-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4715)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.564(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3009(6)
_cell_length_b                   14.0597(6)
_cell_length_c                   14.6315(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2928.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9900
_diffrn_measured_fraction_theta_max 0.9900
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41053
_diffrn_reflns_theta_full        37.1676
_diffrn_reflns_theta_max         37.17
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    4.921
_exptl_crystal_density_diffrn    1.7046
_exptl_crystal_F_000             1461.8651
_refine_diff_density_max         3.0916
_refine_diff_density_min         -2.5607
_refine_diff_density_rms         0.2788
_refine_ls_d_res_high            0.5882
_refine_ls_d_res_low             14.2335
_refine_ls_goodness_of_fit_ref   1.0680
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    61
_refine_ls_number_parameters     322
_refine_ls_number_reflns         14920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0680
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0813
_refine_ls_shift/su_mean         0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+4.0145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12471
_reflns_number_total             14920
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om401063e_si_002.cif
_cod_data_source_block           UMCBTH50
_cod_database_code               4082370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(I2)=1-FVAR(1)
 Sof(N5)=Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(C22)=Sof(H22a)=Sof(H22b)=
 Sof(H22c)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C17(H17a,H17b), C18(H18a,
 H18b), C19(H19a,H19b)
3.b Me refined with riding coordinates:
 C16(H16a,H16b,H16c)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C11(H11), C12(H12)
3.d Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C20(H20a,H20b,
 H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c)
;