A path to improve proton conductivity: from a 3D hydrogen-bonded organic framework to a 3D copper-organic framework
Sun, Zhi-Bing; Li, Yi-Lin; Zhang, Zhe-Hua; Li, Zi-Feng; Xiao, Bo; Li, Gang; New Journal of Chemistry 43 (2019) 10637–; doi:10.1039/C9NJ02025J

data_7058455
_publ_section_title
;
 A path to improve proton conductivity: from a 3D hydrogen-bonded organic
 framework to a 3D copper-organic framework
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10637
_journal_paper_doi               10.1039/C9NJ02025J
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C40 H47 Cu6 N8 O13 S3, 2.75(C H4 O)'
_chemical_formula_sum            'C42.75 H58 Cu6 N8 O15.75 S3'
_chemical_formula_weight         1413.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1ny74z
_audit_creation_date             2019-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-31 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8459(9)
_cell_length_b                   19.8487(5)
_cell_length_c                   25.4804(8)
_cell_measurement_reflns_used    8020
_cell_measurement_temperature    116.6
_cell_measurement_theta_max      29.2570
_cell_measurement_theta_min      3.0789
_cell_volume                     11048.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      116.6
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -5.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000  -90.0000 54

  2 omega   -8.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   77.0000  150.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0296144000
_diffrn_orient_matrix_UB_12      0.0028936000
_diffrn_orient_matrix_UB_13      0.0111539000
_diffrn_orient_matrix_UB_21      -0.0132702000
_diffrn_orient_matrix_UB_22      0.0074174000
_diffrn_orient_matrix_UB_23      0.0247410000
_diffrn_orient_matrix_UB_31      -0.0003886000
_diffrn_orient_matrix_UB_32      -0.0348440000
_diffrn_orient_matrix_UB_33      0.0062257000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33155
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.085
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             5747
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0697P)^2^+43.1867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7470
_reflns_number_total             10465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02025j2.cif
_cod_data_source_block           170418_szb_10
_cod_depositor_comments          'Adding full bibliography for 7058455.cif.'
_cod_database_code               7058455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         c53h36n2o2Cu1
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C32-N8
 1.4 with sigma of 0.02
 H15A-O12
 2.2 with sigma of 0.02
 C33A-C41_$1
 3.4 with sigma of 0.02
 O9-H9
 0.87 with sigma of 0.01
 H41B_$1-H33D
 2.2 with sigma of 0.02
 O16-C43
 1.4 with sigma of 0.02
 O16A-C43A
 1.4 with sigma of 0.02
 C17-H9
 1.910813 with sigma of 0.02
 Cu4-H9
 3.027519 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O13, N8, C32, C31, C33, C32A, N8A, C33A, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16, C43, C43A, O16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(N8A)=Sof(C33A)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C31A)=Sof(H31A)=1-FVAR(1)
 Sof(N8)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31)=Sof(H31)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
 Fixed Sof: O16(0.5) H16(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
 C43A(0.25) H43D(0.25) H43E(0.25) H43F(0.25) O16A(0.25) H16D(0.25)
6.a Riding coordinates:
 O15(H15A), O16(H16), O16A(H16D)
6.b Rotating group:
 O10(H10A,H10B)
6.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C9(H9A,H9B), C20(H20A,H20B)
6.d Aromatic/amide H refined with riding coordinates:
 C28(H28), C31(H31), C11(H11), C15(H15), C35(H35), C39(H39), C12(H12),
 C14(H14), C36(H36), C38(H38), C22(H22), C26(H26), C23(H23), C25(H25),
 C31A(H31A)
6.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C16(H16A,H16B,
 H16C), C40(H40A,H40B,H40C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C27(H27A,
 H27B,H27C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C43A(H43D,H43E,H43F)
6.f Idealised tetrahedral OH refined as rotating group:
 O14(H14A)
;
_shelx_res_checksum              88459
_olex2_submission_special_instructions 'No special instructions were received'