NHC adducts of tantalum amidohalides: the first example of NHC abnormally coordinated to an early transition metal.
Petrov, Pavel A.; Sukhikh, Taisiya S.; Sokolov, Maxim N.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4902–4906; doi:10.1039/c7dt00748e

data_7042382
_publ_section_title
;
 NHC adducts of tantalum amidohalides: the first example of NHC abnormally
 coordinated to an early transition metal.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4902
_journal_page_last               4906
_journal_paper_doi               10.1039/c7dt00748e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C6 H18 Cl3 N3 Ta, C21 H24 N2, C21 H25 N2'
_chemical_formula_sum            'C48 H67 Cl3 N7 Ta'
_chemical_formula_weight         1029.38
_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_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     iterative
_audit_creation_date             2017-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-02 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.091(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5698(11)
_cell_length_b                   26.431(2)
_cell_length_c                   15.2341(13)
_cell_measurement_reflns_used    2481
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.42
_cell_measurement_theta_min      2.31
_cell_volume                     5048.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15752
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        20.981
_diffrn_reflns_theta_max         20.981
_diffrn_reflns_theta_min         1.546
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0604 before and 0.0519 after correction. The Ratio of minimum to maximum transmission is 0.8775. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+32.7170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00748e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7042380--7042383.cif.'
_cod_original_cell_volume        5048.4(8)
_cod_database_code               7042382
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C36(H36), C38(H38), C15(H15), C27(H27), C1(H1), C2(H2), C3(H3),
 C24(H24), C6(H6), C17(H17), C8(H8), C23(H23)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C42(H42A,H42B,H42C), C19(H19A,H19B,H19C), C41(H41A,H41B,
 H41C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C40(H40A,H40B,H40C), C21(H21A,
 H21B,H21C), C31(H31A,H31B,H31C), C12(H12A,H12B,H12C), C62(H62A,H62B,H62C),
 C11(H11A,H11B,H11C), C72(H72A,H72B,H72C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C71(H71A,H71B,H71C), C61(H61A,H61B,H61C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'