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_4082373
_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         'C24 H38 I N8 Ta'
_chemical_formula_sum            'C24 H38 I N8 Ta'
_chemical_formula_weight         746.47
_chemical_name_systematic        TH-6-116
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2012-11-02
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.10.26 svn.r2515, GUI svn.r4371)
;
_cell_angle_alpha                89.884(1)
_cell_angle_beta                 84.039(1)
_cell_angle_gamma                86.730(1)
_cell_formula_units_Z            4
_cell_length_a                   10.6851(12)
_cell_length_b                   10.9572(12)
_cell_length_c                   24.299(3)
_cell_measurement_temperature    100
_cell_volume                     2824.9(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.13
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9108
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34679
_diffrn_reflns_theta_full        29.0552
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    5.010
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7550
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452.5117
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.1540
_refine_diff_density_min         -1.0800
_refine_diff_density_rms         0.1449
_refine_ls_d_res_high            0.7317
_refine_ls_d_res_low             12.0839
_refine_ls_goodness_of_fit_ref   1.1452
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    112
_refine_ls_number_parameters     626
_refine_ls_number_reflns         13751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1452
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.0201
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+6.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                13302
_reflns_number_total             13751
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om401063e_si_002.cif
_cod_data_source_block           UMCB0024_TH_6_116_0m
_cod_original_cell_volume        2824.9(5)
_cod_database_code               4082373
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, {H7a,H7b} of C7, {H8a,H8b} of C8, {H9a,H9b} of C9, H11 of C11,
  H12 of C12, H13 of C13, {H16a,H16b} of C16, {H17a,H17b} of C17, {H18a,H18b}
  of C18, {H33a,H33b} of C33, H20 of C20, {H32a,H32b} of C32, {H34a,H34b} of
  C34, H36 of C36, H37 of C37, H38 of C38, H39 of C39, H42 of C42, {H43a,H43b}
  of C43, {H44a,H44b} of C44, {H45a,H45b} of C45
 At 1.5 times of:
  {H2a,H2b,H2c} of C2, {H10a,H10b,H10c} of C10, {H1a,H1b,H1c} of C1, {H19a,
  H19b,H19c} of C19, {H22a,H22b,H22c} of C22, {H23a,H23b,H23c} of C23, {H24a,
  H24b,H24c} of C24, {H26a,H26b,H26c} of C26, {H27a,H27b,H27c} of C27, {H28a,
  H28b,H28c} of C28, {H35a,H35b,H35c} of C35, {H46a,H46b,H46c} of C46, {H47a,
  H47b,H47c} of C47, {H48a,H48b,H48c} of C48
2.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C16(H16a,H16b), C17(H17a,H17b),
 C18(H18a,H18b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b), C43(H43a,H43b),
  C44(H44a,H44b), C45(H45a,H45b)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C12(H12), C13(H13), C20(H20), C36(H36), C37(H37), C38(H38),
 C39(H39), C42(H42)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C10(H10a,H10b,H10c), C19(H19a,H19b,H19c),
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,
 H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C35(H35a,H35b,H35c), C46(H46a,
 H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c)
;
_shelxl_version_number           2012-9