Robust multifunctional Zr-based metal‒organic polyhedra for high proton conductivity and selective CO2 capture
Xing, Wen-Hao; Li, Hai-Yang; Dong, Xi-Yan; Zang, Shuang-Quan; Journal of Materials Chemistry A 6 (2018) 7724–; doi:10.1039/C8TA00858B

data_7237118
_publ_section_title
;
 Robust multifunctional Zr-based metal--organic polyhedra for high proton
 conductivity and selective CO2 capture
;
_journal_issue                   17
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7724
_journal_paper_doi               10.1039/C8TA00858B
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C78 H73.92 Na3.96 O47.96 S6 Zr6'
_chemical_formula_sum            'C78 H73.92 Na3.96 O47.96 S6 Zr6'
_chemical_formula_weight         2609.37
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-18 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.2679(2)
_cell_length_b                   16.2679(2)
_cell_length_c                   84.1291(12)
_cell_measurement_reflns_used    21931
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.8620
_cell_measurement_theta_min      5.4620
_cell_volume                     19281.5(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -100
_diffrn_reflns_number            17402
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.473
_diffrn_reflns_theta_max         67.473
_diffrn_reflns_theta_min         5.249
_exptl_absorpt_coefficient_mu    5.532
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.79644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             7831
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+83.4355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3527
_reflns_number_total             3873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta00858b2.cif
_cod_data_source_block           MOP-1
_cod_original_cell_volume        19281.5(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7237118
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.608
_shelx_estimated_absorpt_t_min   0.491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B} of O10A, {H9BA,H9BB} of O9B, All C(H,H) groups
 At 1.5 times of:
  {H9AA,H9AB} of O9A, {H10C,H10D} of O10B
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.01
 Na1A-O8
 2.2 with sigma of 0.005
 O10A-Na1A
 2.3 with sigma of 0.01
 Na1B-O10B = Na1B-O9A = Na1B-O8
 2.3 with sigma of 0.01
 H9BB_$1-H4_$2
 2.2 with sigma of 0.01
 H9AB_$1-H4_$2
 2.2 with sigma of 0.01
 S1-O7 \\sim S1-O6 \\sim S1-O8
 with sigma of 0.01
 S1-O6 \\sim S1-O8 \\sim S1-O7
 with sigma of 0.01
 O8-O6 \\sim O6-O7
 with sigma of 0.01
 O8-O7 \\sim O7-O6
 with sigma of 0.01
3. Rigid bond restraints
 O8, O7, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O8 \\sim O6 \\sim O7: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(Zr1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1B) \\sim Ueq, Uanis(Na1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Na1B) \\sim Ueq, Uanis(O10B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Na1B) \\sim Ueq, Uanis(O9A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10A) \\sim Ueq, Uanis(O9B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: Na1A(0.45) O10A(0.2) H10A(0.2) H10B(0.2) O9B(0.2) H9BA(0.2)
 H9BB(0.2) Na1B(0.21) O10B(0.13) H10C(0.13) H10D(0.13) O9A(0.13) H9AA(0.13)
 H9AB(0.13)
6.a Riding coordinates:
 O10A(H10A,H10B), O9B(H9BA,H9BB), O10B(H10C,H10D), O9A(H9AA,H9AB)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C12(H12), C2(H2A), C3(H3), C6(H6), C4(H4), C5(H5)
;
_shelx_res_checksum              14630
_shelx_fab_checksum              77816
_olex2_submission_special_instructions 'No special instructions were received'