Missing metal-linker connectivities in a 3-D robust sulfonate-based metal-organic framework for enhanced proton conductivity.
Zhang, Guiyang; Fei, Honghan; Chemical communications (Cambridge, England) 53 (2017) 4156–4159; doi:10.1039/c7cc01461a

data_7119868
_publ_section_title
;
 Missing metal-linker connectivities in a 3-D robust sulfonate-based
 metal-organic framework for enhanced proton conductivity.
;
_journal_issue                   29
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4156
_journal_page_last               4159
_journal_paper_doi               10.1039/c7cc01461a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C56 H48 Cu2 N8 O13 S4'
_chemical_formula_sum            'C56 H50 Cu2 N8 O13 S4'
_chemical_formula_weight         1298.36
_chemical_name_common            TMOF-2
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6139(12)
_cell_length_b                   15.7965(13)
_cell_length_c                   29.712(2)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.92
_cell_volume                     7328.3(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      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            137753
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.890
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 4529 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         16902
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1019P)^2^+5.9453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                12019
_reflns_number_total             16902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01461a2.cif
_cod_data_source_block           160520a
_cod_depositor_comments          'Adding full bibliography for 7119868.cif.'
_cod_database_code               7119868
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C46(H46A,H46B), C49(H49A,H49B), C54(H54A,H54B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23),
  C22(H22), C21(H21), C24(H24), C27(H27), C29(H29), C28(H28), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40),
  C43(H43), C44(H44), C47(H47), C48(H48), C51(H51), C52(H52), C55(H55), C56(H56)
;
_olex2_submission_special_instructions 'No special instructions were received'