Pyrene and porphyrin-based Zn metal 1-D-polymer: synthesis, molecular structure, and photocatalytic property
Gupta, Gajendra; Kim, Miyeon; Singh, Neetu; Lee, Junseong; Lee, Chang Yeon; Dalton Transactions  (2022) –; doi:10.1039/D2DT00299J

data_7709629
_publ_section_title
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 Pyrene and porphyrin-based Zn metal 1-D-polymer: synthesis, molecular
 structure, and photocatalytic property
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00299J
_journal_year                    2022
_chemical_formula_moiety         'C140 H88 N12 Zn2, 2(C3 N O), 2(C3 H7 N O)'
_chemical_formula_sum            'C152 H102 N16 O4 Zn2'
_chemical_formula_weight         2347.27
_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     iterative
_audit_creation_date             2020-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.889(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2278(13)
_cell_length_b                   20.3428(14)
_cell_length_c                   20.3837(19)
_cell_measurement_reflns_used    8688
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.035
_cell_measurement_theta_min      2.332
_cell_volume                     5899.4(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_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  0.0848
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38331
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.690
_diffrn_reflns_theta_min         2.002
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1314 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.5561.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             2436
_refine_diff_density_max         3.074
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6068
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.1412
_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^)+(0.1292P)^2^+190.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3535
_refine_ls_wR_factor_ref         0.3713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4417
_reflns_number_total             6068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00299j2.cif
_cod_data_source_block           inu62-3
_cod_database_code               7709629
_shelxl_version_number           2014-3
_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
 N6-C43
 1.4 with sigma of 0.02
 N6-C42 = N5-C41 = N6-C44 = N5-C40 = N6-C43 = N5-C39
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C42 \\sim N6 \\sim C44 \\sim C43: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24A) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C39) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C37A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23A) \\sim Ueq, Uanis(C38A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C38(0.75) H38(0.75) C24(0.75) H24(0.75) C23(0.75) H23(0.75)
 C37(0.75) H37(0.75) C24A(0.25) H24A(0.25) C23A(0.25) H23A(0.25) C37A(0.25)
 H37A(0.25) C38A(0.25) H38A(0.25) C42(0.5) N6(0.5) C39(0.5) H39(0.5) O1(0.5)
 O2(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) N5(0.5) C44(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) H41C(0.5) C43(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C7(H7), C15(H15), C12(H12), C18(H18), C27(H27), C8(H8),
 C29(H29), C30(H30), C22(H22), C34(H34), C21(H21), C20(H20), C16(H16), C14(H14),
  C19(H19), C38(H38), C24(H24), C23(H23), C13(H13), C37(H37), C24A(H24A),
 C23A(H23A), C37A(H37A), C38A(H38A), C39(H39)
5.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
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_shelx_res_checksum              74455
_shelx_hkl_checksum              13014
_olex2_submission_special_instructions 'No special instructions were received'