Chlorination of a Pyrazole Ligand in Vanadium(V)alkoxo Complexes1
Holger Glas; Eberhardt Herdtweck; Georg R. J. Artus; Werner R. Thiel; Inorganic Chemistry 37 (1998) 3644–3646; doi:10.1021/ic9715355

data_4322878
_publ_contact_author
;
       Dr. Eberhardt Herdtweck
       Anorganisch-chemisches Institut der
       Technischen Universit\"at M\"unchen
       Lichtenbergstrasse 4
       D-85747 Garching bei M\"unchen
;
_publ_contact_author_email       herdtweck@vogon.anorg.chemie.tu-muenchen.de
_publ_contact_author_fax         ' 089 289 13473'
_publ_contact_author_phone       '089 289 13143'
_publ_section_title
;
 Chlorination of a Pyrazole Ligand in Vanadium(V)alkoxo Complexes1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3644
_journal_page_last               3646
_journal_paper_doi               10.1021/ic9715355
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C16 H21 Cl3 N3 O4 V'
_chemical_formula_weight         476.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.43(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.119(1)
_cell_length_b                   12.095(1)
_cell_length_c                   19.438(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      18.2
_cell_volume                     2093.6(4)
_computing_cell_refinement       STRUX-V
_computing_data_collection       STRUX-V
_computing_data_reduction        STRUX-V
_computing_molecular_graphics    'PLATON PLUTON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(1)
_diffrn_measurement_device       'MACH3 Enraf Nonius'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3890
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        5.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'orange colored'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_obs          0.0375
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+1.5260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1096
_refine_ls_wR_factor_obs         0.1027
_reflns_number_observed          3135
_reflns_number_total             3663
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715355_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+1.5260P] 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^)+(0.0590P)^2^+1.5260P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322878