Single-crystal superprotonic conductivity in an interpenetrated hydrogen-bonded quadruplex framework
Zhou, Mu-Yang; Wang, Hao-Yu; Wang, Zhi-Shuo; Zhang, Xue-Wen; Feng, Xi; Gao, Le-Yao; Lian, Zhi-Cheng; Lin, Rui-Biao; Zhou, Dong-Dong; Chemical Communications  (2021) –; doi:10.1039/D1CC06004J

data_7129340
_publ_section_title
;
 Single-crystal superprotonic conductivity in an interpenetrated
 hydrogen-bonded quadruplex framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06004J
_journal_year                    2021
_chemical_formula_moiety
'0.25(C80 H56 K4 N32 O64), 0.25(H12 O4), 2.5(H2 O)'
_chemical_formula_sum            'C20 H22 K N8 O19.5'
_chemical_formula_weight         725.55
_chemical_name_common            1-H2O
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-10 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5128(5)
_cell_length_b                   27.5128(5)
_cell_length_c                   3.52247(9)
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.2940
_cell_measurement_theta_min      3.2100
_cell_volume                     2666.35(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            9947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.424
_diffrn_reflns_theta_max         67.424
_diffrn_reflns_theta_min         3.212
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.387
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1204
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+22.8458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1094
_reflns_number_total             1204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06004j2.cif
_cod_data_source_block           1-h2o
_cod_original_cell_volume        2666.35(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C20 H22 K N8 O19.50'
_cod_database_code               7129340
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.0000
_shelx_estimated_absorpt_t_min   0.34664
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H2(0.5) O5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) O6(0.3125)
 H6A(0.3125) H6B(0.3125) O7(0.3125) H7A(0.3125) H7B(0.3125)
4.a Riding coordinates:
 O3(H3), N1(H1), N2(H2), O5(H5A,H5B,H5C), O6(H6A,H6B), O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
;
_shelx_res_checksum              73692
_olex2_submission_special_instructions 'No special instructions were received'