Reticular Chemistry at Its Best: Directed Assembly of Hexagonal Building Units into the Awaited Metal-Organic Framework with the Intricate Polybenzene Topology, pbz-MOF.
Alezi, Dalal; Spanopoulos, Ioannis; Tsangarakis, Constantinos; Shkurenko, Aleksander; Adil, Karim; Belmabkhout, Youssef; O Keeffe, Michael; Eddaoudi, Mohamed; Trikalitis, Pantelis N.; Journal of the American Chemical Society 138 (2016) 12767–12770; doi:10.1021/jacs.6b08176

data_4130966
_publ_section_title
;
 Reticular Chemistry at Its Best: Directed Assembly of Hexagonal Building
 Units into the Awaited Metal-Organic Framework with the Intricate
 Polybenzene Topology, pbz-MOF.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12767
_journal_page_last               12770
_journal_paper_doi               10.1021/jacs.6b08176
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C94 H68 O32 Zr6'
_chemical_formula_sum            'C94 H68 O32 Zr6'
_chemical_formula_weight         2256.80
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.856(2)
_cell_length_b                   44.856(2)
_cell_length_c                   44.856(2)
_cell_measurement_reflns_used    1882
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      61.73
_cell_measurement_theta_min      4.29
_cell_volume                     90253(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            30106
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        55.945
_diffrn_reflns_theta_max         55.945
_diffrn_reflns_theta_min         4.296
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  0.2652
_exptl_absorpt_correction_T_min  0.1713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0730 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.6459.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.664
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             18048
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0800
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1755
_reflns_number_total             2761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08176_si_002.cif
_cod_data_source_block           pbz-MOF-1
_cod_original_cell_volume        90252(9)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               4130966
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C2 = C4-C3 = C5-C4 = C7-C6 = C8-C7 = C9-C8
 1.39 with sigma of 0.001
 C11-C12
 1.5 with sigma of 0.01
 Zr1-O3 \\sim Zr1_$2-O3 \\sim Zr1_$1-O3
 with sigma of 0.001
3. Restrained planarity
 C2, C3, C4, C5, C3_$2, C4_$2
 with sigma of 0.001
 C6, C7, C8, C9, C7_$2, C8_$2
 with sigma of 0.001
4. Rigid bond restraints
 O1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O4 \\sim C11 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C3 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.002
Uanis(C10) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6. Others
 Fixed Sof: C11(0.41667) C12(0.41667) H12A(0.41667) H12B(0.41667) H12C(0.41667)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8)
7.b Idealised Me refined with riding coordinates:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              72310
_shelx_hkl_checksum              47192
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'