Mono- and bis-N-heterocyclic carbene complexes of tantalum and niobium with high oxidation states
Wei, ZhenHong; Zhang, Wenbiao; Luo, Guangming; Xu, Feng; Mei, YingXuan; Cai, Hu; New J. Chem. 40 (2016) 6270–; doi:10.1039/C6NJ00223D

data_7055530
_publ_section_title
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 Mono- and bis-N-heterocyclic carbene complexes of tantalum and niobium
 with high oxidation states
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              6270
_journal_paper_doi               10.1039/C6NJ00223D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C42 H48 Cl4 N4 Nb, Cl6 Nb, 4(C H2 Cl2)'
_chemical_formula_sum            'C46 H56 Cl18 N4 Nb2'
_chemical_formula_weight         1488.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-17 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                66.765(3)
_cell_angle_beta                 86.819(4)
_cell_angle_gamma                71.851(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8499(10)
_cell_length_b                   15.0205(10)
_cell_length_c                   16.9789(11)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.827
_cell_measurement_theta_min      2.748
_cell_volume                     3075.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Apex-II CCD diffractometer'
_diffrn_measurement_method       'Thin slice \f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47265
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, v2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.07
_refine_diff_density_min         -1.74
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         14275
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0255P)^2^+18.5287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                11414
_reflns_number_total             14275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj00223d2.cif
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055529--7055531.cif.
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_cod_database_code               7055530