A potential synthon for models of vanadium haloperoxidase: (3,5-dimethylpyrazole)bis[2-hydroxy-2-methylbutanoato(1–)]oxovanadium(IV)
Sara L. Raishbrook; Peter Turner; Rachel Codd; Acta Crystallographica Section E 58 (2002) m737–m739; doi:10.1107/S1600536802020937

data_2201490
_publ_section_title
;
 A potential synthon for models of vanadium haloperoxidase:
 (3,5-dimethylpyrazole)bis[2-hydroxy-2-methylbutanoato(1--)]oxovanadium(IV)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m737
_journal_page_last               m739
_journal_paper_doi               10.1107/S1600536802020937
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[V O (C5 H9 O3)2 (C5 H8 N2)]'
_chemical_formula_moiety         'C15 H26 N2 O7 V'
_chemical_formula_sum            'C15 H26 N2 O7 V'
_chemical_formula_weight         397.32
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.215(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.990(10)
_cell_length_b                   10.140(5)
_cell_length_c                   20.240(10)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.709
_cell_measurement_theta_min      2.847
_cell_volume                     3929(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT and XPREP (Siemens, 1995)'
_computing_molecular_graphics
;
TEXSAN for Windows (Molecular Structure Corporation, 1997),
Xtal3.6 (Hall et al., 1999), ORTEPII  (Johnson, 1976) and WinGX
(Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18722
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.25
_diffrn_standards_number         199
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.186
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.752
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.485
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.539
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.05P)^2^+5P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                3825
_reflns_number_total             4642
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6006.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201490
_cod_database_fobs_code          2201490