Proton conduction in a new 3-D open-framework vanadoborate with an abundant hydrogen bond system
Liu, Xinxin; Zhang, Dan; Li, Lingyun; Sun, Xuejiao; Zhang, Le; Yuan, Hongming; Dalton Transactions 46 (2017) 9103–9109; doi:10.1039/C7DT01334E

data_1546342
_publ_section_title
;
 Proton conduction in a new 3-D open-framework vanadoborate with an
 abundant hydrogen bond system
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              9103
_journal_page_last               9109
_journal_paper_doi               10.1039/C7DT01334E
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'B18 H6 O60 V12, 4(C2 H10 N2), 10(O)'
_chemical_formula_sum            'C8 H46 B18 N8 O70 V12'
_chemical_formula_weight         2180.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.118(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7963(11)
_cell_length_b                   14.7612(8)
_cell_length_c                   21.9272(12)
_cell_measurement_reflns_used    55557
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.730
_cell_measurement_theta_min      2.784
_cell_volume                     7012.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      172.99
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55557
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.730
_diffrn_reflns_theta_min         2.784
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       Rod-Like
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
TITL 1 in C2/c
CELL   22.7963   14.7612   21.9272     90.00    108.12     90.00
SPGR C2/c
C101 0.133 0.261 0.410 !       4.36 eA-3
Q102 0.977 0.307 0.202 !       3.67 eA-3
C103 0.861 0.328 0.128 !       2.55 eA-3
Q104 0.881 0.316 0.152 !       2.31 eA-3
Q105 0.952 0.016 0.321 !       2.02 eA-3
Q106 0.104 0.221 0.389 !       2.01 eA-3
Q107 0.872 0.251 0.207 !       1.87 eA-3
Q108 0.937 0.153 0.223 !       1.75 eA-3
Q109 0.774 0.233 0.003 !       1.74 eA-3
Q110 0.798 0.296 0.148 !       1.56 eA-3
Q111 0.108 0.183 0.037 !       1.30 eA-3
Q112 0.388 0.461 0.302 !       1.28 eA-3
Q113 0.789 0.234 0.071 !       1.20 eA-3
Q114 0.046 0.217 0.326 !       1.20 eA-3
Q115 0.201 0.374 0.325 !       0.72 eA-3
Q116 0.586 0.172 0.140 !       0.71 eA-3
Q117 0.228 0.208 0.154 !       0.68 eA-3
Q118 0.889 0.234 0.157 !       0.67 eA-3
Q119 1.000 0.250 0.251 !       0.65 eA-3
Q120 0.386 0.107 0.048 !       0.63 eA-3
Q121 0.767 0.499 0.475 !       0.60 eA-3
Q122 0.313 0.252 0.290 !       0.58 eA-3
Q123 0.881 0.333 0.192 !       0.56 eA-3
Q124 0.055 0.136 0.075 !       0.55 eA-3
Q125 0.249 0.020 0.094 !       0.54 eA-3
Q126 0.740 0.247 0.079 !       0.54 eA-3
Q127 0.385 0.170 0.424 !       0.53 eA-3
Q128 0.301 0.093 0.358 !       0.53 eA-3
Q129 0.959 0.130 0.169 !       0.53 eA-3
Q130 0.304 0.230 0.350 !       0.52 eA-3
Q131 0.681 0.123 0.196 !       0.51 eA-3
;
_refine_diff_density_max         1.894
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6645
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+83.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5805
_reflns_number_total             6645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01334e2.cif
_cod_data_source_block           1
_cod_database_code               1546342
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H23 of O23, {H2A,H2B,H2C} of N2, {H3A,H3B,H3C} of N3,
  {H4A,H4B,H4C} of N4
 At 1.5 times of:
  H21 of O21, H29 of O29, {H1A1,H1A2,H1A3} of N1A, {H1B1,H1B2,H1B3} of N1B
2. Restrained distances
 C2-C1A = C4-C3
 1.47 with sigma of 0.02
 N3-C3 = N4-C4 = N2-C2 = N1A-C1A
 1.53 with sigma of 0.02
 N2-C1A
 2.47 with sigma of 0.02
 C2-N1A
 2.47 with sigma of 0.02
 N3-C4
 2.47 with sigma of 0.02
 C3-N4
 2.47 with sigma of 0.02
 N2-N1A
 3.76 with sigma of 0.02
 N3-N4
 3.76 with sigma of 0.02
 O23-O24
 2.38 with sigma of 0.02
 N1A-C1A
 1.53 with sigma of 0.02
 C2-C1A
 1.47 with sigma of 0.02
 C1B-C2
 1.47 with sigma of 0.02
 N1B-C1B
 1.53 with sigma of 0.02
 C2-N1B
 2.4 with sigma of 0.02
 O23-H23
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: C1A(0.65) H1A4(0.65) H1A5(0.65) C1B(0.35) H1B4(0.35) H1B5(0.35)
 N1A(0.65) H1A1(0.65) H1A2(0.65) H1A3(0.65) N1B(0.35) H1B1(0.35) H1B2(0.35)
 H1B3(0.35)
4.a Rotating group:
 O23(H23)
4.b Secondary CH2 refined with riding coordinates:
 C1A(H1A4,H1A5), C1B(H1B4,H1B5), C3(H3D,H3E), C4(H4D,H4E)
4.c Idealised Me refined as rotating group:
 N1A(H1A1,H1A2,H1A3), N1B(H1B1,H1B2,H1B3), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C),
 N4(H4A,H4B,H4C)
4.d Idealised tetrahedral OH refined as rotating group:
 O21(H21), O29(H29)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'