Porphyrin Metal-Organic Frameworks with Bilayer and Pillar-layered Frameworks for Third-order Nonlinear Optical Properties
Zhu, Zi-Yi; Wang, Zirui; Li, Qiao-Hong; Ma, Zhi-Zhou; Wang, Fei; Zhang, Jian; Dalton Transactions  (2023) –; doi:10.1039/D3DT00440F

data_7712651
_publ_section_title
;
 Porphyrin Metal-Organic Frameworks with Bilayer and Pillar-layered
 Frameworks for Third-order Nonlinear Optical Properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00440F
_journal_year                    2023
_chemical_formula_moiety         'C64 H34 N8 O8 Zn3'
_chemical_formula_sum            'C64 H34 N8 O8 Zn3'
_chemical_formula_weight         1239.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-09 deposited with the CCDC.	2023-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5128(4)
_cell_length_b                   23.5272(3)
_cell_length_c                   18.2894(3)
_cell_measurement_reflns_used    17656
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      60.3780
_cell_measurement_theta_min      2.3230
_cell_volume                     10047.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     17.00  71.00   0.50    1.53    --   -1.25  24.00  43.00  108
  2  \w    -72.00 -30.00   0.50    1.53    --   -1.25 -24.00-120.00   84
  3  \w    -23.00   3.00   0.50    1.53    --   -1.25 -24.00-120.00   52
  4  \w     58.00 143.00   0.50    6.30    --   72.27  24.00  43.00  170
  5  \w     -4.00  73.00   0.50    6.30    --   72.27 -24.00-120.00  154
  6  \w   -140.00 -92.00   0.50    6.30    --  -74.77 -24.00-120.00   96
  7  \w    -12.00  38.00   0.50    1.53    --   -1.25  57.00-180.00  100
  8  \w      0.00  87.00   0.50    6.30    --   72.27 -57.00-180.00  174
  9  \w      1.00  81.00   0.50    6.30    --   72.27 -57.00 150.00  160
 10  \w    -75.00 -20.00   0.50    6.30    --  -74.77 125.00  60.00  110
 11  \w   -147.00 -87.00   0.50    6.30    --  -74.77-125.00   0.00  120
 12  \w   -106.00 -63.00   0.50    6.30    --  -74.77 125.00 120.00   86
 13  \w    -48.00 -22.00   0.50    6.30    --  -74.77 125.00 120.00   52
 14  \w   -104.00 -79.00   0.50    6.30    --  -74.77 125.00  60.00   50
 15  \w    -49.00 -24.00   0.50    6.30    --  -74.77  24.00  43.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0395914000
_diffrn_orient_matrix_UB_12      0.0140526000
_diffrn_orient_matrix_UB_13      0.0557581000
_diffrn_orient_matrix_UB_21      -0.0374038000
_diffrn_orient_matrix_UB_22      -0.0111399000
_diffrn_orient_matrix_UB_23      0.0479543000
_diffrn_orient_matrix_UB_31      0.0180248000
_diffrn_orient_matrix_UB_32      -0.0540410000
_diffrn_orient_matrix_UB_33      0.0046009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33925
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.318
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.819
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.219
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8770
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.534
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0815
_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^)+(0.1433P)^2^+37.5876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7601
_reflns_number_total             8770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00440f2.cif
_cod_data_source_block           ZnTCPP-2
_cod_database_code               7712651
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C N O'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.929
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Zn02) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 Zn02, Zn01, N007, O003, C00M, C00U, C00C, C00K, N00A, C00T, C019, C00D, H00K,
 C01A, H019, C01B, C00Y, H01A, C01C, H01B, C00W, H00Y, H01C, C00I, H00W, C014,
 C011, N00B, C016, C015, H016, C018, N008, C010, H018, C00G, C00S, C00V, C00L,
 C00N, C00O, C00X, C013, C00E, H00N, H00O, H00X, C012, C00Z, H013, C00P, H012,
 C00Q, H00Z, H00P, C00R, C00H, C00J, H00R, O004, O005, C00F, O006
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Zn02, C014, C00I, C00W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C00O(H00O), C00P(H00P), C00R(H00R), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C012(H012), C013(H013), C016(H016),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61261
_shelx_fab_checksum              15965
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.223
_oxdiff_exptl_absorpt_empirical_full_min 0.479