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_5000405
_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         '5(C8 H20 N 1+), O36 V15 5-, 1.28(C2 H3 N)'
_chemical_formula_sum            'C42.56 H103.84 N6.28 O36 V15'
_chemical_formula_weight         2043.92
_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                 107.560(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.105(3)
_cell_length_b                   13.7840(19)
_cell_length_c                   26.604(4)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    101
_cell_measurement_theta_max      15.77
_cell_measurement_theta_min      10.8
_cell_volume                     7728.4(18)
_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  0.064
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13681
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        0.9
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.8029
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4143
_exptl_crystal_size_max          .56
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .14
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.97
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       0.3841E-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   2.5203
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4190
_refine_ls_R_factor_gt           0.1111
_refine_ls_shift/su_max          0.2286
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.05F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                4190
_reflns_number_total             6847
_reflns_threshold_expression     F^2^>2.33\s(F^2^)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               5000405