#------------------------------------------------------------------------------
#$Date: 2020-09-06 12:31:48 +0300 (Sun, 06 Sep 2020) $
#$Revision: 256059 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704914.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704914
loop_
_publ_author_name
'Zhang, Shi-Hui'
'Zhang, Shu-Yu'
'Li, Jing-Rong'
'Huang, Zhen-Qi'
'Yang, Jing'
'Yue, Ke-Fen'
'Wang, Yao-Yu'
_publ_section_title
;
 Rational synthesis of an ultra-stable Zn(ii) coordination polymer based
 on a new tripodal pyrazole ligand for the highly sensitive and selective
 detection of Fe³⁺ and Cr₂O₇²⁻
 in aqueous media.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11201
_journal_page_last               11208
_journal_paper_doi               10.1039/d0dt01996h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H16 N6 O6 Zn'
_chemical_formula_sum            'C24 H16 N6 O6 Zn'
_chemical_formula_weight         549.80
_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   mixed
_audit_creation_date             2018-04-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-11-21 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.520(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0291(19)
_cell_length_b                   8.3132(10)
_cell_length_c                   17.158(2)
_cell_measurement_reflns_used    3592
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.37
_cell_volume                     2285.6(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12356
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.783
_diffrn_reflns_theta_min         2.375
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0636 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.8924. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0348
_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/[σ²(Fo²)+(0.0445P)²+0.3940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3819
_reflns_number_total             4807
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01996h2.cif
_cod_data_source_block           xb9884_0m_shelxl
_cod_depositor_comments          'Adding full bibliography for 7704914.cif.'
_cod_original_cell_volume        2285.5(5)
_cod_database_code               7704914
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), N11(H11), C14(H14), C17(H17), C18(H18), C22(H22), C23(H23), C28(H28),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
2.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.80059(2) 0.15173(3) 0.23047(2) 0.02983(10) Uani 1 1 d . . . . .
O5 O 0.89552(10) 0.0094(2) 0.19965(10) 0.0405(4) Uani 1 1 d . . . . .
N1 N 0.69453(11) 0.0416(2) 0.26095(11) 0.0331(4) Uani 1 1 d . . . . .
N3 N 0.76875(12) 0.3682(2) 0.18926(12) 0.0348(5) Uani 1 1 d . . . . .
O3 O 1.02453(12) 0.1170(2) 0.66178(10) 0.0476(5) Uani 1 1 d . . . . .
H3 H 1.0443 0.1000 0.7056 0.071 Uiso 1 1 calc GR . . . .
O1 O 0.84947(10) 0.2273(2) 0.32957(9) 0.0381(4) Uani 1 1 d . . . . .
C4 C 0.78006(17) 0.5084(3) 0.22515(15) 0.0430(6) Uani 1 1 d . . . . .
H4 H 0.8162 0.5248 0.2677 0.052 Uiso 1 1 calc R . . . .
N5 N 0.36800(13) -0.3470(3) 0.48151(13) 0.0425(5) Uani 1 1 d . . . . .
N2 N 0.68904(12) -0.0014(3) 0.33619(12) 0.0336(5) Uani 1 1 d . . . . .
C9 C 0.42707(14) -0.3318(3) 0.53762(14) 0.0326(5) Uani 1 1 d . . . . .
O2 O 0.82128(11) 0.0777(2) 0.43280(10) 0.0485(5) Uani 1 1 d . . . . .
N11 N 0.71195(12) 0.3979(2) 0.13129(11) 0.0341(5) Uani 1 1 d . . . . .
H11 H 0.6936 0.3265 0.0988 0.041 Uiso 1 1 calc R . . . .
C12 C 0.61377(14) -0.0610(3) 0.35194(14) 0.0329(5) Uani 1 1 d . . . . .
C13 C 0.86518(14) 0.1742(3) 0.39743(14) 0.0312(5) Uani 1 1 d . . . . .
C14 C 0.99693(14) 0.3283(3) 0.39063(13) 0.0307(5) Uani 1 1 d . . . . .
H14 H 0.9807 0.3550 0.3398 0.037 Uiso 1 1 calc R . . . .
C15 C 0.94442(14) 0.2350(3) 0.43549(13) 0.0293(5) Uani 1 1 d . . . . .
C16 C 1.04494(14) 0.2501(3) 0.54241(13) 0.0326(5) Uani 1 1 d . . . . .
C17 C 1.09666(15) 0.3425(3) 0.49662(14) 0.0342(5) Uani 1 1 d . . . . .
H17 H 1.1476 0.3785 0.5171 0.041 Uiso 1 1 calc R . . . .
C18 C 0.52261(14) -0.1986(3) 0.44672(14) 0.0333(5) Uani 1 1 d . . . . .
H18 H 0.4866 -0.2283 0.4058 0.040 Uiso 1 1 calc R . . . .
C19 C 0.50401(14) -0.2424(3) 0.52243(13) 0.0307(5) Uani 1 1 d . . . . .
O4 O 1.14097(13) 0.2609(3) 0.65033(11) 0.0625(6) Uani 1 1 d . . . . .
C21 C 0.59428(14) -0.1108(3) 0.43108(14) 0.0324(5) Uani 1 1 d . . . . .
C22 C 0.56819(16) -0.0570(4) 0.28273(14) 0.0440(6) Uani 1 1 d . . . . .
H22 H 0.5134 -0.0909 0.2744 0.053 Uiso 1 1 calc R . . . .
C23 C 0.55876(14) -0.1990(3) 0.58332(14) 0.0328(5) Uani 1 1 d . . . . .
H23 H 0.5474 -0.2295 0.6341 0.039 Uiso 1 1 calc R . . . .
C24 C 0.87213(15) -0.0190(3) 0.12957(14) 0.0348(5) Uani 1 1 d . . . . .
C25 C 1.07558(17) 0.2124(3) 0.62301(14) 0.0401(6) Uani 1 1 d . . . . .
O6 O 0.80535(11) 0.0385(2) 0.10394(10) 0.0498(5) Uani 1 1 d . . . . .
N6 N 0.30801(14) -0.4364(3) 0.51471(14) 0.0485(6) Uani 1 1 d . . . . .
C28 C 0.40310(17) -0.4090(4) 0.60514(16) 0.0499(7) Uani 1 1 d . . . . .
H28 H 0.4329 -0.4146 0.6523 0.060 Uiso 1 1 calc R . . . .
C29 C 1.07311(14) 0.3818(3) 0.42065(14) 0.0324(5) Uani 1 1 d . . . . .
C30 C 0.63020(14) -0.1104(3) 0.56857(13) 0.0318(5) Uani 1 1 d . . . . .
C31 C 0.96834(14) 0.1963(3) 0.51145(13) 0.0304(5) Uani 1 1 d . . . . .
H31 H 0.9334 0.1345 0.5418 0.037 Uiso 1 1 calc R . . . .
C32 C 0.64774(14) -0.0673(3) 0.49295(14) 0.0342(5) Uani 1 1 d . . . . .
H32 H 0.6957 -0.0085 0.4832 0.041 Uiso 1 1 calc R . . . .
C33 C 0.62061(15) 0.0075(3) 0.22840(15) 0.0408(6) Uani 1 1 d . . . . .
H33 H 0.6061 0.0247 0.1762 0.049 Uiso 1 1 calc R . . . .
C34 C 0.32677(18) -0.4751(4) 0.58814(17) 0.0535(8) Uani 1 1 d . . . . .
H34 H 0.2943 -0.5353 0.6215 0.064 Uiso 1 1 calc R . . . .
C35 C 0.73101(18) 0.6264(3) 0.19081(16) 0.0455(7) Uani 1 1 d . . . . .
H35 H 0.7279 0.7339 0.2054 0.055 Uiso 1 1 calc R . . . .
C36 C 0.68781(14) 0.5526(3) 0.13070(13) 0.0324(5) Uani 1 1 d . . . . .
H6 H 0.264(2) -0.456(4) 0.4822(19) 0.074(10) Uiso 1 1 d . . . . .
H2 H 0.7301(18) 0.015(3) 0.3692(17) 0.058(9) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Zn1 N1 116.84(8) . . ?
O5 Zn1 O6 58.80(6) . . ?
N1 Zn1 O6 96.06(7) . . ?
N3 Zn1 O5 128.78(8) . . ?
N3 Zn1 N1 107.00(8) . . ?
N3 Zn1 O6 92.73(7) . . ?
O1 Zn1 O5 97.43(7) . . ?
O1 Zn1 N1 103.99(7) . . ?
O1 Zn1 N3 96.38(8) . . ?
O1 Zn1 O6 154.41(7) . . ?
C24 O5 Zn1 98.72(14) . . ?
N2 N1 Zn1 116.61(14) . . ?
C33 N1 Zn1 137.64(17) . . ?
C33 N1 N2 105.47(19) . . ?
C4 N3 Zn1 126.63(17) . . ?
C4 N3 N11 105.15(19) . . ?
N11 N3 Zn1 125.88(15) . . ?
C13 O1 Zn1 138.90(16) . . ?
N3 C4 C35 110.9(2) . . ?
C9 N5 N6 104.3(2) . . ?
C12 N2 N1 112.00(19) . . ?
N5 C9 C19 120.1(2) . . ?
N5 C9 C28 110.5(2) . . ?
C28 C9 C19 129.4(2) . . ?
C36 N11 N3 111.62(19) . . ?
N2 C12 C21 120.6(2) . . ?
N2 C12 C22 106.1(2) . . ?
C22 C12 C21 133.3(2) . . ?
O1 C13 C15 115.4(2) . . ?
O2 C13 O1 125.2(2) . . ?
O2 C13 C15 119.4(2) . . ?
C29 C14 C15 120.9(2) . . ?
C14 C15 C13 117.7(2) . . ?
C31 C15 C13 122.7(2) . . ?
C31 C15 C14 119.5(2) . . ?
C17 C16 C25 117.1(2) . . ?
C17 C16 C31 119.6(2) . . ?
C31 C16 C25 123.4(2) . . ?
C29 C17 C16 120.7(2) . . ?
C19 C18 C21 121.1(2) . . ?
C18 C19 C9 120.0(2) . . ?
C18 C19 C23 119.1(2) . . ?
C23 C19 C9 120.8(2) . . ?
C18 C21 C12 121.7(2) . . ?
C18 C21 C32 118.9(2) . . ?
C32 C21 C12 119.4(2) . . ?
C12 C22 C33 105.8(2) . . ?
C30 C23 C19 120.4(2) . . ?
O5 C24 C29 119.0(2) . 2_745 ?
O6 C24 O5 119.5(2) . . ?
O6 C24 C29 121.5(2) . 2_745 ?
O3 C25 C16 113.4(2) . . ?
O4 C25 O3 123.0(2) . . ?
O4 C25 C16 123.5(2) . . ?
C24 O6 Zn1 82.93(15) . . ?
C34 N6 N5 112.8(2) . . ?
C34 C28 C9 105.9(2) . . ?
C14 C29 C17 119.3(2) . . ?
C14 C29 C24 119.2(2) . 2_755 ?
C17 C29 C24 121.5(2) . 2_755 ?
C23 C30 C36 123.0(2) . 4_566 ?
C32 C30 C23 119.8(2) . . ?
C32 C30 C36 117.1(2) . 4_566 ?
C15 C31 C16 120.1(2) . . ?
C30 C32 C21 120.7(2) . . ?
N1 C33 C22 110.6(2) . . ?
N6 C34 C28 106.5(2) . . ?
C36 C35 C4 105.9(2) . . ?
N11 C36 C30 119.5(2) . 4_565 ?
N11 C36 C35 106.4(2) . . ?
C35 C36 C30 133.9(2) . 4_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O5 2.0094(16) . ?
Zn1 N1 2.0120(19) . ?
Zn1 N3 1.9946(19) . ?
Zn1 O1 1.9568(16) . ?
Zn1 O6 2.3692(18) . ?
O5 C24 1.272(3) . ?
N1 N2 1.345(3) . ?
N1 C33 1.327(3) . ?
N3 C4 1.328(3) . ?
N3 N11 1.353(3) . ?
O3 C25 1.330(3) . ?
O1 C13 1.264(3) . ?
C4 C35 1.380(3) . ?
N5 C9 1.338(3) . ?
N5 N6 1.353(3) . ?
N2 C12 1.338(3) . ?
C9 C19 1.469(3) . ?
C9 C28 1.388(3) . ?
O2 C13 1.237(3) . ?
N11 C36 1.343(3) . ?
C12 C21 1.461(3) . ?
C12 C22 1.378(3) . ?
C13 C15 1.500(3) . ?
C14 C15 1.392(3) . ?
C14 C29 1.386(3) . ?
C15 C31 1.387(3) . ?
C16 C17 1.389(3) . ?
C16 C25 1.489(3) . ?
C16 C31 1.398(3) . ?
C17 C29 1.386(3) . ?
C18 C19 1.389(3) . ?
C18 C21 1.393(3) . ?
C19 C23 1.394(3) . ?
O4 C25 1.206(3) . ?
C21 C32 1.394(3) . ?
C22 C33 1.380(3) . ?
C23 C30 1.390(3) . ?
C24 O6 1.242(3) . ?
C24 C29 1.495(3) 2_745 ?
N6 C34 1.327(3) . ?
C28 C34 1.365(4) . ?
C29 C24 1.495(3) 2_755 ?
C30 C32 1.382(3) . ?
C30 C36 1.472(3) 4_566 ?
C35 C36 1.372(3) . ?
C36 C30 1.472(3) 4_565 ?
