Towards hydroperoxovanadium complexes: the X-ray crystal structure of a peroxovanadium(v) complex containing a V(O2)(RCO2H)(H2O)2 cluster with hydrogen bond inter-linkages
Časný, Marian; Rehder, Dieter; Chemical Communications  (2001) 921–; doi:10.1039/b101010g

data_7114847
_publ_section_title
;
 Towards hydroperoxovanadium complexes: the X-ray crystal structure of a
 peroxovanadium(v) complex containing a V(O2)(RCO2H)(H2O)2 cluster with
 hydrogen bond inter-linkages
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              921
_journal_paper_doi               10.1039/b101010g
_journal_year                    2001
_chemical_formula_sum            'C15 H21 Cl N3 O11 V'
_chemical_formula_weight         505.74
_chemical_name_systematic
; 
N,N-bis(2-pyridylmethyl)-beta-alanine-oxo-peroxovanadium 
perchlorate dihydrate 
;
_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                 123.274(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.612(7)
_cell_length_b                   7.1835(17)
_cell_length_c                   21.290(5)
_cell_measurement_reflns_used    4382
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.54
_cell_volume                     4042.0(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11777
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9343
_exptl_absorpt_correction_T_min  0.8745
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                3378
_reflns_number_total             4382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101010g.txt
_cod_data_source_block           m3arian
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4042.1(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7114847