First Non-Centrosymmetric Deca-Vanadoborate with Borate Vacancies, Self-Assembled around a 1,3-Propanediammonium Cation
Muñoz-Becerra, Karina; Hermosilla-Ibáñez, Patricio; Le Fur, Eric; Cador, Olivier; Paredes-García, Verónica; Spodine, Evgenia; Venegas-Yazigi, Diego; Crystal Growth & Design 15 (2015) 2561–; doi:10.1021/acs.cgd.5b00102

data_4513011
_publ_section_title
;
 First Non-Centrosymmetric Deca-Vanadoborate with Borate Vacancies,
 Self-Assembled around a 1,3-Propanediammonium Cation
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2561
_journal_paper_doi               10.1021/acs.cgd.5b00102
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety
(NH3CH2CH2CH2NH3)6[V10B24O66H8]&#x00E2;&#x0088;&#x0099;13.23H2O
_chemical_formula_sum            'C18 H80 B24 N12 O79.23 V10'
_chemical_formula_weight         2501.46
_chemical_name_systematic
; 
 ? 
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3012(2)
_cell_length_b                   16.5873(2)
_cell_length_c                   17.1743(2)
_cell_measurement_reflns_used    46617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4643.81(10)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46881
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.949
_diffrn_standards_number         46881
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2511.6
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0505
_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^)+(0.1032P)^2^+0.5900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                8542
_reflns_number_total             10714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00102_si_002.cif
_cod_data_source_block           Compound(1)_Venegas-Yazigi
_cod_depositor_comments          'Adding full bibliography for 4513011.cif.'
_cod_database_code               4513011