Naphthalene-1,8-dicarboxylate based zinc coordination polymers: a photophysical study
Guerrero-García, Pablo; Cepeda, Javier; Ortega-Muñoz, Mariano; García, Jose Angel; Navarro, Amparo; Choquesillo-Lazarte, Duane; Rojas, Sara; Diéguez, Antonio Rodríguez; Quesada-Moreno, María Mar; Vitórica-Yrezábal, Iñigo J.; CrystEngComm 26 (2024) 1268–1277; doi:10.1039/D3CE01233F

data_7248050
_publ_section_title
;
 Naphthalene-1,8-dicarboxylate based zinc coordination polymers: a
 photophysical study
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1268
_journal_page_last               1277
_journal_paper_doi               10.1039/D3CE01233F
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C17 H11 N O8 Zn, C3 H7 N O'
_chemical_formula_sum            'C20 H18 N2 O9 Zn'
_chemical_formula_weight         495.73
_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             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-03 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.569(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.361(4)
_cell_length_b                   5.9049(6)
_cell_length_c                   21.101(2)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.64
_cell_measurement_theta_min      4.65
_cell_volume                     4086.9(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Apex3, 2019'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16962
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.813
_diffrn_reflns_theta_max         66.813
_diffrn_reflns_theta_min         4.646
_exptl_absorpt_coefficient_mu    2.189
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4901
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1218 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.6510.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3559
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+6.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3378
_reflns_number_total             3559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01233f2.cif
_cod_data_source_block           pg111
_cod_depositor_comments
'Adding full bibliography for 7248050--7248052.cif.'
_cod_original_cell_volume        4086.8(7)
_cod_database_code               7248050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.779
_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
 N2-C16 \\sim N2A-C16A
 with sigma of 0.02
 N4-C19 \\sim N4-C1A
 with sigma of 0.02
 N2-C15 \\sim N2A-C15A
 with sigma of 0.02
 N2-C17 \\sim N2A-C17A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.04
 O8-N2 \\sim O8A-N2A
 with sigma of 0.04
 C16-C17 \\sim C16A-C17A
 with sigma of 0.04
 N1-C1C \\sim N1-C1D
 with sigma of 0.02
 Zn1-O8 \\sim Zn1-O8A
 with sigma of 0.02
 O8-C15 \\sim O8A-C15A
 with sigma of 0.02
 Zn1-C15 \\sim Zn1-C15A
 with sigma of 0.04
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
3. Restrained planarity
 C18, O9, N4, C19, C1A
 with sigma of 0.1
 C1B, O10, N1, C1C, C1D
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O8 \\sim N2 \\sim C15 \\sim C16 \\sim C17 \\sim O8A \\sim C15A \\sim N2A \\sim
C17A \\sim C16A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C18 \\sim O9 \\sim N4 \\sim C19 \\sim C1A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C1B \\sim O10 \\sim N1 \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C18 \\sim O9 \\sim N4 \\sim C19 \\sim C1A \\sim C1B \\sim O10 \\sim N1 \\sim
C1C \\sim C1D: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C16 \\sim C16A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.04 within 2A
Uanis(C16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.04
Uanis(C16) = Uanis(C16A)
5. Rigid body (RIGU) restrains
 O8A, N2A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, O9, N4, C19, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, N4, C18, O9, C1A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O8, N2, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, O10, N1, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C18, O9, N4, C19, C1B, O10, N1, C1C, C1D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(O8A)=Sof(C15A)=Sof(H15A)=Sof(N2A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(O8)=Sof(N2)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(C1B)=Sof(H1B)=Sof(O10)=Sof(N1)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(2)
 Sof(C18)=Sof(H18)=Sof(O9)=Sof(N4)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(2)
7.a Free rotating group:
 C18(O9,N4,C19,C1A), C1B(O10,N1,C1C,C1D)
7.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C16A(H16D,
 H16E,H16F), C19(H19A,H19B,H19C), C1A(H1AA,H1AB,H1AC), C1C(H1CA,H1CB,H1CC),
 C1D(H1DA,H1DB,H1DC)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C15(H15), C15A(H15A), C18(H18), C1B(H1B)
;
_shelx_res_checksum              81776
_shelx_hkl_checksum              79072
_olex2_submission_special_instructions 'No special instructions were received'