Creating Well-Defined Hexabenzocoronene in Zirconium Metal-Organic Framework by Postsynthetic Annulation.
Qin, Jun-Sheng; Yuan, Shuai; Zhang, Lei; Li, Bao; Du, Dong-Ying; Huang, Ning; Guan, Wei; Drake, Hannah F.; Pang, Jiandong; Lan, Ya-Qian; Alsalme, Ali; Zhou, Hong-Cai; Journal of the American Chemical Society 141 (2019) 2054–2060; doi:10.1021/jacs.8b11042

data_4133552
_publ_section_title
;
 Creating Well-Defined Hexabenzocoronene in Zirconium Metal-Organic
 Framework by Postsynthetic Annulation.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2054
_journal_page_last               2060
_journal_paper_doi               10.1021/jacs.8b11042
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.06(C1344 H576 O512 Zr96)'
_chemical_formula_sum            'C84 H36 O32 Zr6'
_chemical_formula_weight         2104.45
_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
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.655(10)
_cell_length_b                   44.655
_cell_length_c                   44.655
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.762
_cell_measurement_theta_min      2.799
_cell_volume                     89045(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.762
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0944 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.7602.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.628
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             16576
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         6.112
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.744
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         3841
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.941
_refine_ls_R_factor_all          0.1856
_refine_ls_R_factor_gt           0.1625
_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          0.4203
_refine_ls_wR_factor_ref         0.4359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2732
_reflns_number_total             3841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11042_si_001.cif
_cod_data_source_block           PCN-136
_cod_original_cell_volume        89045(6)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               4133552
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-Zr1_$1
 2.18 with sigma of 0.005
 C9-C8
 1.4 with sigma of 0.005
 C7-C7_$2
 2.2 with sigma of 0.005
 C8-C8_$2
 2.2 with sigma of 0.005
 C8_$2-C8_$3
 1.4 with sigma of 0.005
 C6-C5
 1.5 with sigma of 0.005
 C10_$4-C10
 1.4 with sigma of 0.005
 C9-C10
 1.4 with sigma of 0.005
 C8_$2-C7_$2
 1.4 with sigma of 0.005
 C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C7-C6 \\sim C8-C7 \\sim C9-C8 \\sim C9-C10
 with sigma of 0.02
 C6-C5 \\sim C2-C1
 with sigma of 0.02
 C8-C7 \\sim C9-C8 \\sim C9-C8_$2 \\sim C8_$2-C7_$2 \\sim C7_$2-C6 \\sim C7-C6
 with sigma of 0.02
3. Restrained planarity
 C9, C8, C7, C6, C7_$2, C8_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4) = Uanis(O3) = Uanis(O2) = Uanis(O1)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C4(H4)
;
_shelx_res_checksum              9411
_shelx_hkl_checksum              6341
_olex2_submission_special_instructions 'No special instructions were received'