Mononuclear oxovanadium complexes of tris(2-pyridylmethyl)amine.
Tajika, Yasunobu; Tsuge, Kiyoshi; Sasaki, Yoichi; Dalton transactions (Cambridge, England : 2003)  (2005) 1438–1447; doi:10.1039/b414532a

data_7007974
_publ_section_title
;
 Mononuclear oxovanadium complexes of tris(2-pyridylmethyl)amine.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1438
_journal_page_last               1447
_journal_paper_doi               10.1039/b414532a
_journal_year                    2005
_chemical_formula_sum            'C18.5 H23 Cl N4 O5 V'
_chemical_formula_weight         467.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.7140(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.0018(2)
_cell_length_b                   16.064(2)
_cell_length_c                   28.6544(9)
_cell_measurement_reflns_used    8801
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.1016
_cell_measurement_theta_min      1.9265
_cell_volume                     4057.3(5)
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    MULTAN88
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 7.3153
_diffrn_measured_fraction_theta_full 0.0000
_diffrn_measured_fraction_theta_max 27.1016
_diffrn_measurement_details
;
scan:
Number of images: 360
Slice: -70.0000 - 110.0000
Image width: 0.5000
Exp time: 60.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 50.4576
2theta: 20.0013
scan:
Number of images: 120
Slice: -10.0000 - 50.0000
Image width: 0.5000
Exp time: 60.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 50.4576
2theta: 20.0013

;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           Molybdenum
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.1016
_diffrn_reflns_theta_max         27.1016
_diffrn_reflns_theta_min         1.9265
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  1.0066
_exptl_absorpt_correction_T_min  0.7514
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.750
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7970
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                6464
_reflns_number_total             7970
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b414532a.txt
_cod_data_source_block           '[V(O)(O2)(tpa)]Cl'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C18.50 H23 Cl N4 O5 V '
_cod_database_code               7007974
_diffrn_number_total             17669
_diffrn_reflns_av_sigmai/deti    0.0926