Synthesis and X-ray characterization of a monomeric Cp-free d1-imido‒vanadium(IV) complex
Lorber, Christian; Donnadieu, Bruno; Choukroun, Robert; Journal of the Chemical Society, Dalton Transactions  (2000) 4497–; doi:10.1039/b008761k

data_7010416
_publ_section_title
;
 Synthesis and X-ray characterization of a monomeric Cp-free
 d1-imido--vanadium(IV) complex
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4497
_journal_paper_doi               10.1039/b008761k
_journal_year                    2000
_chemical_formula_sum            'C16 H31 Cl2 N3 V'
_chemical_formula_weight         387.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.099(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6595(13)
_cell_length_b                   9.7366(10)
_cell_length_c                   20.783(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.45
_cell_volume                     2100.9(4)
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean '(1.45 - 24.2)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany'
_diffrn_measurement_method       'rotation en ?'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\?
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1369
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11827
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped_exptl_crystal_colour
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.40mm
_exptl_crystal_size_mid          0.35mm
_exptl_crystal_size_min          0.20mm
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+3.1224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                2357
_reflns_number_total             2995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008761k.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '160(2)K' was changed to
'160(2)' - the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '160(2)K' was
changed to '160(2)' - the value should be numeric and without a unit
designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7010416
_d(hkl)_range                    '(12.453 - 0.809) '