Pentakis(<small>L</small>-prolinium) dodecatungstoborate trihydrate
Raissi Shabari, Akbar; Pourayoubi, Mehrdad; Ghamari, Dena; Acta Crystallographica Section E 65 (2009) m1586–; doi:10.1107/S1600536809047357

data_2224477
_publ_section_title
;
 Pentakis(<small>L</small>-prolinium) dodecatungstoborate trihydrate
;
_journal_coeditor_code           WM2266
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1586
_journal_paper_doi               10.1107/S1600536809047357
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C5 H10 N O2)5 [B W12 O40], 3H2 O'
_chemical_formula_moiety         '5(C5 H10 N O2 +), B O40 W12 5-, 3(H2 O)'
_chemical_formula_sum            'C25 H56 B N5 O53 W12'
_chemical_formula_weight         3491.76
_chemical_name_systematic
;
Pentakis(L-prolinium) dodecatungstoborate trihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.9135(3)
_cell_length_b                   21.6013(5)
_cell_length_c                   22.2343(5)
_cell_measurement_reflns_used    1485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6202.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0779
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            95451
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    22.273
_exptl_absorpt_correction_T_max  0.110
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6232
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.365
_refine_diff_density_min         -1.042
_refine_ls_abs_structure_details 'Flack (1983), 7492 Friedel pairs'
_refine_ls_abs_structure_Flack   0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         16473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.06P)^2^+1.7105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                15774
_reflns_number_total             16473
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2266.cif
_cod_data_source_block           I
_cod_database_code               2224477
_cod_database_fobs_code          2224477