NMR and X-ray diffraction studies of the complexation of D-(‒)quinic acid with tungsten(vi) and molybdenum(vi)
Ramos, M. Luísa; Pereira, Mariette M.; Beja, Ana Matos; Silva, Manuela R.; Paixão, José A.; Gil, Victor M. S.; Journal of the Chemical Society, Dalton Transactions  (2002) 2126–; doi:10.1039/b109564c

data_7011257
_publ_section_title
;
 NMR and X-ray diffraction studies of the complexation of D-(--)quinic
 acid with tungsten(vi) and molybdenum(vi)
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2126
_journal_paper_doi               10.1039/b109564c
_journal_year                    2002
_chemical_formula_sum            'C14 H29 K2 O18.5 W'
_chemical_formula_weight         755.42
_chemical_name_systematic
; 
potassium bis-quinato tungstate hydrate 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8239(13)
_cell_length_b                   17.772(2)
_cell_length_c                   8.217(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.07
_cell_measurement_theta_min      5.44
_cell_volume                     2456.8(12)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'profile data from \w-2\q 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4914
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.125
_exptl_absorpt_correction_T_max  0.9154
_exptl_absorpt_correction_T_min  0.7921
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North, A.C., Phillips, D.C. & Mattews, F.S. (1968). Acta Cryst., A24,
351-359.
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+11.5538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                4016
_reflns_number_total             4300
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b109564c.txt
_cod_data_source_block           tun
_cod_original_sg_symbol_H-M      P21212
_cod_original_formula_sum        'C14 H29 K2 O18.50 W'
_cod_database_code               7011257