Stable coordination complexes of α-diimines with Nb(v) and Ta(v) halides.
Bartalucci, Niccolò; Bortoluzzi, Marco; Pampaloni, Guido; Pinzino, Calogero; Zacchini, Stefano; Marchetti, Fabio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3346–3355; doi:10.1039/c8dt00122g

data_7045585
_publ_section_title
;
 Stable coordination complexes of \a-diimines with Nb(v) and Ta(v)
 halides.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3346
_journal_page_last               3355
_journal_paper_doi               10.1039/c8dt00122g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C23 H29 Cl6 N2 Nb'
_chemical_formula_weight         639.09
_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_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-22 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                85.466(3)
_cell_angle_beta                 88.650(3)
_cell_angle_gamma                83.733(3)
_cell_formula_units_Z            2
_cell_length_a                   10.004(2)
_cell_length_b                   10.785(3)
_cell_length_c                   12.934(3)
_cell_measurement_reflns_used    4339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.502
_cell_measurement_theta_min      2.3795
_cell_volume                     1382.7(6)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13141
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.646
_diffrn_reflns_theta_min         1.580
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1051 (selected reflections only, before parameter refinement)
 R(int) =  0.0471 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.6164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3866
_reflns_number_total             5167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00122g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045585--7045593.cif.'
_cod_database_code               7045585
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.853
_shelx_res_checksum              73932