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_7007972
_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            'C20 H21 Cl F6 N5 O P V'
_chemical_formula_weight         578.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 99.0217(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.797(2)
_cell_length_b                   14.829(2)
_cell_length_c                   14.162(2)
_cell_measurement_reflns_used    7316
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      30.0326
_cell_measurement_theta_min      1.3730
_cell_volume                     2446.8(6)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 77.4000
_diffrn_measured_fraction_theta_max 30.0326
_diffrn_measurement_details
;
scan:
Number of images: 360
Slice: -76.0000 - 104.0000
Image width: 0.5000
Exp time: 30.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 40.3773
2theta: 14.2496
scan:
Number of images: 120
Slice: -16.0000 - 44.0000
Image width: 0.5000
Exp time: 30.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 40.3773
2theta: 14.2496
;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0526
_diffrn_orient_matrix_UB_12      -0.0214
_diffrn_orient_matrix_UB_13      0.0644
_diffrn_orient_matrix_UB_21      -0.0133
_diffrn_orient_matrix_UB_22      -0.0652
_diffrn_orient_matrix_UB_23      -0.0108
_diffrn_orient_matrix_UB_31      0.0610
_diffrn_orient_matrix_UB_32      -0.0063
_diffrn_orient_matrix_UB_33      -0.0368
_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  0.0160
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15597
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.0326
_diffrn_reflns_theta_max         30.0326
_diffrn_reflns_theta_min         2.0908
_diffrn_source_current           50.0000
_diffrn_source_power             2.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5527
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.484
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5472
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                4377
_reflns_number_total             5472
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b414532a.txt
_cod_data_source_block           '[V(O)Cl(tpa)](PF6)'
_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        'C20 H21 Cl F6 N5 O P V '
_cod_database_code               7007972
_diffrn_number_total             15597
_diffrn_reflns_av_sigmai/deti    0.0508