Creating Giant Secondary Building Layers via Alkali-Etching Exfoliation for Precise Synthesis of Metal‒Organic Frameworks
Li, Lan; Yi, Jun-Dong; Fang, Zhi-Bin; Wang, Xu-Sheng; Liu, Nan; Chen, Ya-Nan; Liu, Tian-Fu; Cao, Rong; Chemistry of Materials 31 (2019) 7584–; doi:10.1021/acs.chemmater.9b02375

data_4003052
_publ_section_title
;
 Creating Giant Secondary Building Layers via Alkali-Etching Exfoliation
 for Precise Synthesis of Metal--Organic Frameworks
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7584
_journal_paper_doi               10.1021/acs.chemmater.9b02375
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         '0.13(C160 H96 N72 O32 Zn16)'
_chemical_formula_sum            'C11.75 H11.75 N11.75 O11.75 Zn11.75'
_chemical_formula_weight         1273.68
_chemical_name_systematic        PFC-17
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-04
_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            8
_cell_length_a                   13.3591(19)
_cell_length_b                   13.3591(19)
_cell_length_c                   42.446(5)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.36
_cell_volume                     7575.1(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            24110
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.321
_diffrn_reflns_theta_min         2.156
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.351
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0817 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.8026. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             4888
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.761
_refine_diff_density_min         -1.820
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0846
_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^)+(0.0717P)^2^+125.5598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2140
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3133
_reflns_number_total             3509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b02375_si_002.cif
_cod_data_source_block           mo_68301_0m_a_sq
_cod_original_cell_volume        7575(2)
_cod_database_code               4003052
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.527
_shelx_estimated_absorpt_t_min   0.307
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 N2, C1, N1, N1_$1, C1_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(N3)
Uanis(N2) = Uanis(N1)
Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C2) = Uanis(C4) = Uanis(C3)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C6(H6), C7(H7), C3(H3), C4(H4)
4.b Fitted hexagon refined as free rotating group:
 C5(C6,C7,C2,C3,C4)
;
_shelx_res_checksum              26696
_shelx_hkl_checksum              86934
_shelx_fab_checksum              235
_olex2_submission_special_instructions 'No special instructions were received'