Stepwise assembly of a polyoxovanadate from mononuclear units in an organic solvent: carboxylate-stabilised fragments in the conversion of [VOCl4]2− to [V15O36]5−
Karet, Gail B.; Streib, William E.; Bollinger, John C.; Christou, George; Sun, Ziming; Hendrickson, David N.; Chemical Communications  () 2249–2250; doi:10.1039/a906448f

data_5000311
_publ_section_title
;
 Stepwise assembly of a polyoxovanadate from mononuclear units in an
 organic solvent: carboxylate-stabilised fragments in the conversion of
 [VOCl4]2&#x2212; to [V15O36]5&#x2212;
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2249
_journal_page_last               2250
_journal_paper_doi               10.1039/a906448f
_chemical_formula_moiety
'(C8 H20 N 1+)2, C8 H12 Cl O17 V5 2-, C2 H3 N'
_chemical_formula_sum            'C26 H55 Cl N3 O17 V5'
_chemical_formula_weight         971.893
_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'
_cell_angle_alpha                90
_cell_angle_beta                 91.390(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.111(2)
_cell_length_b                   14.9003(19)
_cell_length_c                   33.674(5)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    101
_cell_measurement_theta_max      16.86
_cell_measurement_theta_min      12.73
_cell_volume                     8081(3)
_diffrn_ambient_temperature      101
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            7969
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        -3.8
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.2490
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            Blue-green
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          .72
_exptl_crystal_size_mid          .64
_exptl_crystal_size_min          .24
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       0.4152E-7
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.3432
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6432
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.1347
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0411
_reflns_number_gt                6432
_reflns_number_total             7133
_reflns_threshold_expression     F>3.0\s(F)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C26 H55 Cl1 N3 O17 V5'
_cod_database_code               5000311