A tale of hydrogen abstraction, initially detected <i>via</i> X-ray diffraction
Hui, Alice K.; Chen, Chun-Hsing; Terwilliger, Adam M.; Lord, Richard L.; Caulton, Kenneth G.; Acta Crystallographica Section C 70 (2014) 250–255; doi:10.1107/S2053229614003234

data_2019495
_publ_section_title
;
 A tale of hydrogen abstraction, initially detected <i>via</i> X-ray
 diffraction
;
_journal_coeditor_code           FA3324
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              250
_journal_page_last               255
_journal_paper_doi               10.1107/S2053229614003234
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[V (C11 H10 N9) Cl2 O] , 2.5C2 H3 N'
_chemical_formula_moiety         'C11 H10 Cl2 N9 O V, 2.5(C2 H3 N)'
_chemical_formula_sum            'C16 H17.5 Cl2 N11.5 O V'
_chemical_formula_weight         508.755
_chemical_name_systematic
;
Dichlorido[3-methyl-6-[6-(6-methyl-2,3-dihydro-1,2,4,5-tetrazin-3-yl-\
\k<i>N</i>^4^)pyridin-2-yl-\k<i>N</i>]-1,4-dihydro-1,2,4,5-tetrazin-1-\
yl-\k<i>N</i>^1^]oxidovanadium(IV)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1651(5)
_cell_length_b                   23.7109(14)
_cell_length_c                   11.8159(7)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.25
_cell_volume                     2279.6(2)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59575
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.9956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.539
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         14694
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.6092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                12834
_reflns_number_total             14694
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3324sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C16 H17.5 Cl2 N11.5 O1 V1'
_cod_database_code               2019495
_cod_database_fobs_code          2019495