Copper pyrazole directed crystallization of decavanadates: synthesis and characterization of {Cu(pz)}4[{Cu(pz)3}2V10O28] and (Hpz)2[{Cu(pz)4}2V10O28]·2H2O
Thomas, Jency; Agarwal, Monika; Ramanan, Arunachalam; Chernova, Natasha; Whittingham, M. Stanley; CrystEngComm 11 (2009) 625–; doi:10.1039/b815840a

data_7200429
_publ_section_title
;
 Copper pyrazole directed crystallization of decavanadates: synthesis
 and characterization of {Cu(pz)}4[{Cu(pz)3}2V10O28] and
 (Hpz)2[{Cu(pz)4}2V10O28]&#x00B7;2H2O
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              625
_journal_paper_doi               10.1039/b815840a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         '2(C9 H12 Cu N6 O14 V5), C12 H16 Cu N8'
_chemical_formula_sum            'C30 H40 Cu3 N20 O28 V10'
_chemical_formula_weight         1828.87
_chemical_name_common
;tetra(pyrazole)copper(ii)(tri(pyrazole)copper(ii))
decavanadate
;
_chemical_name_systematic
;
tetra(pyrazole)copper(ii)(tri(pyrazole)copper(ii)) decavanadate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.226(2)
_cell_angle_beta                 105.549(3)
_cell_angle_gamma                118.571(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6713(16)
_cell_length_b                   11.9766(16)
_cell_length_c                   12.9000(17)
_cell_measurement_reflns_used    5730
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.18
_cell_volume                     1422.6(3)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16775
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.756
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             901
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0358P)^2^+1.9358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                6111
_reflns_number_total             7081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815840a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               7200429