Synthesis and characterization of d0 imido complexes of vanadium. Crystal structure of [V(2,6-iPr2C6H3N)(S2CNC4H4)3]
Montilla, Francisco; Pastor, Antonio; Monge, Angeles; Gutiérrez-Puebla, Enrique; Galindo, Agustín; Journal of the Chemical Society, Dalton Transactions  (1999) 2893–; doi:10.1039/a903507i

data_7027517
_publ_section_title
;
 Synthesis and characterization of d0 imido complexes of vanadium. Crystal
 structure of [V(2,6-iPr2C6H3N)(S2CNC4H4)3]
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2893
_journal_paper_doi               10.1039/a903507i
_journal_year                    1999
_chemical_formula_sum            'C27 H29 N4 S6 V'
_chemical_formula_weight         652.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.690(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.913(3)
_cell_length_b                   10.0434(12)
_cell_length_c                   27.989(3)
_cell_measurement_temperature    148(2)
_cell_volume                     6977.4(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      148(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1321
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7735
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.213
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_restrained_S_obs      1.213
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_obs          0.0782
_refine_ls_shift/esd_max         -0.024
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2374
_refine_ls_wR_factor_obs         0.2087
_reflns_number_observed          2266
_reflns_number_total             4005
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903507isup1.cif
_cod_data_source_block           pmr14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6977.4(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7027517