Three-Dimensional Metal-Catecholate Frameworks and Their Ultrahigh Proton Conductivity.
Nguyen, Nhung T. T.; Furukawa, Hiroyasu; Gándara, Felipe; Trickett, Christopher A.; Jeong, Hyung Mo; Cordova, Kyle E.; Yaghi, Omar M.; Journal of the American Chemical Society 137 (2015) 15394–15397; doi:10.1021/jacs.5b10999

data_4124754
_publ_section_title
;
 Three-Dimensional Metal-Catecholate Frameworks and Their Ultrahigh Proton
 Conductivity.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15394
_journal_page_last               15397
_journal_paper_doi               10.1021/jacs.5b10999
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'0.25(C192 H240 Fe16 N24 O78.94 S6.94), C4 O0.57'
_chemical_formula_sum            'C52 H60 Fe4 N6 O20.33 S1.73'
_chemical_formula_weight         1373.20
_chemical_name_common            Fe-CAT-420
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8048(5)
_cell_length_b                   17.8048(5)
_cell_length_c                   17.8048(5)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.765
_cell_measurement_theta_min      2.494
_cell_volume                     5644.3(3)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
Diamond - Crystal and Molecular Structure Visualization
Crystal Impact - Dr. H. Putz & Dr. K. Brandenburg GbR, Kreuzherrenstr. 
102, 53227 Bonn, Germany
http://www.crystalimpact.com/diamond
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56833
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_min         2.160
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1396 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.9124.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       Octahedral
_exptl_crystal_F_000             2833
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.826
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1944
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1014P)^2^+23.4252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1578
_reflns_number_total             1944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10999_si_002.cif
_cod_data_source_block           cat-420
_cod_depositor_comments          'Adding full bibliography for 4124754.cif.'
_cod_original_cell_volume        5644.3(5)
_cod_database_code               4124754
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8A-N1
 1.45 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N1, C7, C8B, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S1)=Sof(O5)=FVAR(1)
 Fixed Sof: O3(0.5) O4(0.5) H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) C4AA(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD)
5.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8B(H8BA,H8BB,H8BC), C8A(H8AA,H8AB,H8AC)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
;
_shelx_res_checksum              60726
_shelx_hkl_checksum              51106