Synthesis, characterization, DFT calculations, and reactivity study of a nitrido-bridged dimeric vanadium(iv) complex.
Lugosan, Adriana; Cundari, Thomas; Fleming, Kristin; Dickie, Diane A.; Zeller, Matthias; Ghannam, Jack; Lee, Wei-Tsung; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1200–1206; doi:10.1039/c9dt04544a

data_7703002
_publ_section_title
;
 Synthesis, characterization, DFT calculations, and reactivity study of a
 nitrido-bridged dimeric vanadium(iv) complex.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1200
_journal_page_last               1206
_journal_paper_doi               10.1039/c9dt04544a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H40 Cl2 N5 V, C7 H8'
_chemical_formula_sum            'C39 H48 Cl2 N5 V'
_chemical_formula_weight         708.66
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-27 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6135(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5972(2)
_cell_length_b                   14.7064(3)
_cell_length_c                   21.9685(5)
_cell_measurement_reflns_used    54489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.256
_cell_measurement_theta_min      6.091
_cell_volume                     3728.83(13)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54489
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.256
_diffrn_reflns_theta_min         6.091
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    3.796
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
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_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00115(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0481P)^2^+2.7433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6843
_reflns_number_total             7200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04544a2.cif
_cod_data_source_block           JG-V
_cod_depositor_comments
'Adding full bibliography for 7702999--7703002.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7703002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.489
_shelx_estimated_absorpt_t_max   0.582
_shelx_res_checksum              17520