A zinc(II) triazolate framework with luminescence response toward dichromate anion in aqueous solution
Zou, Ji-Yong; Li, Ling; You, Sheng-Yong; Zhang, Shao-Wei; Inorganica Chimica Acta 498 (2019) 119126–; doi:10.1016/j.ica.2019.119126

data_1565752
_publ_section_title
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 A zinc(II) triazolate framework with luminescence response toward
 dichromate anion in aqueous solution
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_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119126
_journal_paper_doi               10.1016/j.ica.2019.119126
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C14 H14 N18 O4 Zn4'
_chemical_formula_sum            'C14 H14 N18 O4 Zn4'
_chemical_formula_weight         759.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 119.707(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9827(14)
_cell_length_b                   7.6423(5)
_cell_length_c                   20.1616(10)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.517
_cell_measurement_theta_min      3.243
_cell_volume                     2674.3(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.908
_exptl_absorpt_coefficient_mu    3.604
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0849 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.8432.
The \l/2 correction factor is Not present.
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_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.349
_refine_diff_density_min         -3.000
_refine_diff_density_rms         0.321
_refine_ls_extinction_coef       0.0183(14)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4693
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1294P)^2^+41.0482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3011
_reflns_number_total             4693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119126.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1565752
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.548
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C1
 2.2 with sigma of 0.02
 O4-C14
 1.2 with sigma of 0.02
 C14-O3
 1.24 with sigma of 0.02
 C5-C6
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N14)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(N5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Zn4A)=1-FVAR(1)
 Sof(Zn4)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4), C5(H5), C9(H9), C8(H8), C7(H7), C12(H12), C11(H11),
 C10(H10), C3(H3), C1(H1), C13(H13), C14(H14)
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