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_7712650
_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         'C60 H40 N6 O11 Zn3, C4 H8 O2'
_chemical_formula_sum            'C64 H48 N6 O13 Zn3'
_chemical_formula_weight         1305.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-08
_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                118.127(4)
_cell_angle_beta                 90.188(3)
_cell_angle_gamma                108.145(3)
_cell_formula_units_Z            2
_cell_length_a                   16.6123(5)
_cell_length_b                   16.6936(6)
_cell_length_c                   16.7212(6)
_cell_measurement_reflns_used    12636
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9050
_cell_measurement_theta_min      2.7880
_cell_volume                     3823.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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    -63.00  29.00   1.00    1.00    --  -41.54  57.00 150.00   92
  2  \w   -113.00 -17.00   1.00    1.00    --  -41.54 -57.00   0.00   96
  3  \w      8.00  61.00   1.00    1.00    --   41.54 -99.00-150.00   53
  4  \w     82.00 113.00   1.00    1.00    --   41.54  38.00  60.00   31
  5  \w     56.00  82.00   1.00    1.00    --   41.54 -99.00 -90.00   26
  6  \w     20.00  83.00   1.00    1.00    --   41.54  57.00 -60.00   63
  7  \w     49.00 109.00   1.00    1.00    --  108.23-111.00-150.00   60
  8  \w     34.00 110.00   1.00    1.00    --  108.23 -30.00-150.00   76
  9  \w    109.00 159.00   1.00    1.00    --  108.23 111.00 150.00   50
 10  \w     62.00  87.00   1.00    1.00    --  108.23 178.00  30.00   25
 11  \w     99.00 124.00   1.00    1.00    --  108.23 178.00  30.00   25
 12  \w     56.00 109.00   1.00    1.00    --  108.23-111.00   0.00   53
 13  \w     99.00 141.00   1.00    1.00    --  108.23 -77.00 120.00   42
 14  \w     40.00 109.00   1.00    1.00    --  108.23-111.00 120.00   69
 15  \w    109.00 135.00   1.00    1.00    --  108.23  77.00 -60.00   26
 16  \w    106.00 177.00   1.00    1.00    --  108.23 111.00 120.00   71
 17  \w     67.00  97.00   1.00    1.00    --  108.23-111.00  60.00   30
 18  \w     61.00 103.00   1.00    1.00    --  108.23-111.00 -60.00   42
 19  \w     84.00 168.00   1.00    1.00    --  108.23  45.00-120.00   84
 20  \w     53.00  79.00   1.00    1.00    --  108.23 -77.00 120.00   26
 21  \w    111.00 166.00   1.00    1.00    --  108.23 111.00-180.00   55
 22  \w     33.00 136.00   1.00    1.00    --  108.23 -30.00  60.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0785816000
_diffrn_orient_matrix_UB_12      -0.0477949000
_diffrn_orient_matrix_UB_13      -0.0771045000
_diffrn_orient_matrix_UB_21      -0.0602832000
_diffrn_orient_matrix_UB_22      0.0061294000
_diffrn_orient_matrix_UB_23      0.0708284000
_diffrn_orient_matrix_UB_31      0.0054798000
_diffrn_orient_matrix_UB_32      0.1010233000
_diffrn_orient_matrix_UB_33      0.0177149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28712
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.036
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (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    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         15324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0966P)^2^+18.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12699
_reflns_number_total             15324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00440f2.cif
_cod_data_source_block           zzy-7-2-2
_cod_database_code               7712650
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C N O'
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-H4B
 0.856 with sigma of 0.02
3.a Riding coordinates:
 O4(H4A,H4B)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C57(H57A,H57B), C29(H29A,H29B), C59(H59A,H59B), C15(H15A,H15B),
 C61(H61A,H61B), C31(H31A,H31B), C63(H63A,H63B)
3.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C14(H14), C20(H20), C26(H26), C36(H36), C40(H40), C44(H44), C46(H46),
 C50(H50), C54(H54), C58(H58), C60(H60), C62(H62), C64(H64), C9(H9), C39(H39),
 C5(H5A), C21(H21), C43(H43), C11(H11), C45(H45), C47(H47), C3(H3), C49(H49),
 C25(H25), C51(H51), C13(H13), C53(H53), C27(H27), C55(H55)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82792
_shelx_fab_checksum              16525
_olex2_date_sample_data_collection 2021-06-27
_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 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.735