#------------------------------------------------------------------------------
#$Date: 2020-03-07 04:34:16 +0200 (Sat, 07 Mar 2020) $
#$Revision: 249163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/00/7240077.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_7240077
loop_
_publ_author_name
'Kang, Kaijin'
'Meng, Xianghe'
'Liang, Fei'
'Tang, Jian'
'Zeng, Tixian'
'Yin, Wenlong'
'Lin, Zheshuai'
'Xia, Mingjun'
_publ_section_title
;
 Hydroisocyanurates X2Y(H2C3N3O3)4•4H2O (X = K, Cs; Y = Zn, Cd)
 with large birefringence stemming from π−conjugated
 (H2C3N3O3)− anions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00094A
_journal_year                    2020
_chemical_formula_moiety         '0.5(C24 H32 K4 N24 O32 Zn2)'
_chemical_formula_sum            'C12 H16 K2 N12 O16 Zn'
_chemical_formula_weight         727.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-17 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.846(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7653(6)
_cell_length_b                   15.9132(8)
_cell_length_c                   6.9886(3)
_cell_measurement_reflns_used    5021
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      3.2660
_cell_volume                     1167.41(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (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  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6563
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             736
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0326P)²+0.5161P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                1183
_reflns_number_total             1239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce00094a2.cif
_cod_data_source_block           k2zn
_cod_original_cell_volume        1167.41(10)
_cod_database_code               7240077
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z'
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
K1 K 0.14468(4) 0.5000 0.36744(8) 0.02648(14) Uani 1 d . . 2 S T P
Zn1 Zn 0.5000 0.5000 0.5000 0.01620(13) Uani 1 d . . 4 S T P
C1 C 0.60344(12) 0.68103(8) 0.5147(2) 0.0145(3) Uani 1 d . . 1 . . .
C2 C 0.39950(12) 0.31564(9) -0.0062(2) 0.0156(3) Uani 1 d . . 1 . . .
C3 C 0.5000 0.81520(12) 0.5000 0.0179(4) Uani 1 d . . 2 S T P
C4 C 0.5000 0.18206(12) 0.0000 0.0185(4) Uani 1 d . . 2 S T P
O1 O 0.70084(9) 0.64674(6) 0.52930(17) 0.0214(2) Uani 1 d . . 1 . . .
O2 O 0.40768(14) 0.5000 0.7050(2) 0.0213(3) Uani 1 d . . 2 S T P
O3 O 0.30478(9) 0.35178(6) -0.01044(17) 0.0226(2) Uani 1 d . . 1 . . .
O4 O 0.32386(14) 0.5000 0.2095(2) 0.0214(3) Uani 1 d . . 2 S T P
O5 O 0.5000 0.89196(9) 0.5000 0.0283(4) Uani 1 d . . 2 S T P
O6 O 0.5000 0.10529(9) 0.0000 0.0288(4) Uani 1 d . . 2 S T P
N1 N 0.5000 0.63749(10) 0.5000 0.0148(3) Uani 1 d . . 2 S T P
N2 N 0.5000 0.35885(10) 0.0000 0.0171(3) Uani 1 d . . 2 S T P
N3 N 0.59967(10) 0.76810(7) 0.51125(19) 0.0181(3) Uani 1 d . . 1 . . .
H3 H 0.6649 0.7943 0.5166 0.022 Uiso 1 calc . . 1 R . .
N4 N 0.40082(10) 0.22897(7) -0.00735(19) 0.0187(3) Uani 1 d . . 1 . . .
H4A H 0.3353 0.2029 -0.0130 0.022 Uiso 1 calc . . 1 R . .
H2 H 0.4251(19) 0.4559(13) 0.779(3) 0.039(5) Uiso 1 d . . 1 . . .
H4 H 0.319(2) 0.4587(13) 0.134(4) 0.055(7) Uiso 1 d . . 1 . . .
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'
K K 0.2009 0.2494 '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
K1 K1 K1 97.971(17) 5_566 5_565 ?
Zn1 K1 K1 115.715(16) . 5_565 ?
Zn1 K1 K1 146.314(19) . 5_566 ?
O1 K1 K1 109.94(2) 2_656 5_565 ?
O1 K1 K1 109.94(2) 5_666 5_565 ?
O1 K1 K1 113.98(2) 5_666 5_566 ?
O1 K1 K1 113.98(2) 2_656 5_566 ?
O1 K1 Zn1 55.90(2) 2_656 . ?
O1 K1 Zn1 55.90(2) 5_666 . ?
O1 K1 O1 110.34(4) 2_656 5_666 ?
O1 K1 O2 58.21(2) 2_656 . ?
O1 K1 O2 58.21(2) 5_666 . ?
O1 K1 O5 144.99(3) 5_666 7_566 ?
O1 K1 O5 144.99(3) 2_656 3_445 ?
O1 K1 O5 80.18(3) 5_666 3_445 ?
O1 K1 O5 80.18(3) 2_656 7_566 ?
O1 K1 O6 138.92(3) 5_666 3_455 ?
O1 K1 O6 138.92(3) 2_656 7 ?
O1 K1 O6 78.58(3) 5_666 7 ?
O1 K1 O6 78.58(3) 2_656 3_455 ?
O2 K1 K1 112.66(3) . 5_566 ?
O2 K1 K1 149.37(3) . 5_565 ?
O2 K1 Zn1 33.66(3) . . ?
O4 K1 K1 82.62(3) . 5_565 ?
O4 K1 K1 179.40(4) . 5_566 ?
O4 K1 Zn1 33.09(3) . . ?
O4 K1 O1 65.76(3) . 2_656 ?
O4 K1 O1 65.76(3) . 5_666 ?
O4 K1 O2 66.75(4) . . ?
O4 K1 O5 142.93(2) . 3_445 ?
O4 K1 O5 142.93(2) . 7_566 ?
O4 K1 O6 84.00(3) . 7 ?
O4 K1 O6 84.00(3) . 3_455 ?
O5 K1 K1 96.353(14) 3_445 5_565 ?
O5 K1 K1 37.07(2) 7_566 5_566 ?
O5 K1 K1 96.353(14) 7_566 5_565 ?
O5 K1 K1 37.07(2) 3_445 5_566 ?
O5 K1 Zn1 131.602(19) 3_445 . ?
O5 K1 Zn1 131.602(19) 7_566 . ?
O5 K1 O2 107.90(3) 3_445 . ?
O5 K1 O2 107.90(3) 7_566 . ?
O5 K1 O5 74.13(5) 3_445 7_566 ?
O5 K1 O6 74.97(2) 3_445 7 ?
O5 K1 O6 74.97(2) 7_566 3_455 ?
O5 K1 O6 116.08(2) 7_566 7 ?
O5 K1 O6 116.08(2) 3_445 3_455 ?
O6 K1 K1 96.488(14) 7 5_566 ?
O6 K1 K1 96.488(14) 3_455 5_566 ?
O6 K1 K1 35.44(2) 3_455 5_565 ?
O6 K1 K1 35.44(2) 7 5_565 ?
O6 K1 Zn1 110.702(13) 7 . ?
O6 K1 Zn1 110.702(13) 3_455 . ?
O6 K1 O2 134.51(3) 3_455 . ?
O6 K1 O2 134.51(3) 7 . ?
O6 K1 O6 70.88(5) 7 3_455 ?
K1 Zn1 K1 180.0 5_666 . ?
O2 Zn1 K1 131.20(4) 5_666 . ?
O2 Zn1 K1 131.20(4) . 5_666 ?
O2 Zn1 K1 48.80(4) 5_666 5_666 ?
O2 Zn1 K1 48.80(4) . . ?
O2 Zn1 O2 180.0 . 5_666 ?
O2 Zn1 N1 90.0 5_666 5_666 ?
O2 Zn1 N1 90.0 . . ?
O2 Zn1 N1 90.0 5_666 . ?
O2 Zn1 N1 90.0 . 5_666 ?
O4 Zn1 K1 45.08(4) . . ?
O4 Zn1 K1 134.92(4) . 5_666 ?
O4 Zn1 K1 45.08(4) 5_666 5_666 ?
O4 Zn1 K1 134.92(4) 5_666 . ?
O4 Zn1 O2 86.12(6) 5_666 . ?
O4 Zn1 O2 93.88(6) . . ?
O4 Zn1 O2 93.88(6) 5_666 5_666 ?
O4 Zn1 O2 86.12(6) . 5_666 ?
O4 Zn1 O4 179.999(1) . 5_666 ?
O4 Zn1 N1 90.0 . . ?
O4 Zn1 N1 90.0 5_666 . ?
O4 Zn1 N1 90.0 . 5_666 ?
O4 Zn1 N1 90.0 5_666 5_666 ?
N1 Zn1 K1 90.0 . 5_666 ?
N1 Zn1 K1 90.0 5_666 . ?
N1 Zn1 K1 90.0 . . ?
N1 Zn1 K1 90.0 5_666 5_666 ?
N1 Zn1 N1 180.0 5_666 . ?
O1 C1 N1 123.15(13) . . ?
O1 C1 N3 117.75(12) . . ?
N1 C1 N3 119.09(12) . . ?
O3 C2 N2 121.84(13) . . ?
O3 C2 N4 118.36(12) . . ?
N2 C2 N4 119.80(12) . . ?
O5 C3 N3 123.34(8) . . ?
O5 C3 N3 123.34(8) . 2_656 ?
N3 C3 N3 113.32(16) . 2_656 ?
O6 C4 N4 123.11(8) . . ?
O6 C4 N4 123.11(8) . 2_655 ?
N4 C4 N4 113.78(17) . 2_655 ?
C1 O1 K1 148.10(9) . 5_666 ?
K1 O2 H2 111.8(14) . . ?
Zn1 O2 K1 97.55(5) . . ?
Zn1 O2 H2 110.8(14) . . ?
K1 O4 H4 114.3(15) . . ?
Zn1 O4 K1 101.83(6) . . ?
Zn1 O4 H4 111.0(17) . . ?
K1 O5 K1 105.87(5) 3 7_566 ?
C3 O5 K1 127.07(2) . 3 ?
C3 O5 K1 127.07(2) . 7_566 ?
K1 O6 K1 109.13(5) 7 3_545 ?
C4 O6 K1 125.44(2) . 7 ?
C4 O6 K1 125.44(2) . 3_545 ?
C1 N1 Zn1 120.54(8) 2_656 . ?
C1 N1 Zn1 120.54(8) . . ?
C1 N1 C1 118.92(16) 2_656 . ?
C2 N2 C2 118.84(17) 2_655 . ?
C1 N3 H3 117.6 . . ?
C3 N3 C1 124.77(12) . . ?
C3 N3 H3 117.6 . . ?
C2 N4 H4A 118.1 . . ?
C4 N4 C2 123.89(12) . . ?
C4 N4 H4A 118.1 . . ?
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
K1 K1 4.7090(10) 5_565 ?
K1 K1 4.5520(9) 5_566 ?
K1 Zn1 3.8518(5) . ?
K1 O1 2.8448(10) 5_666 ?
K1 O1 2.8448(10) 2_656 ?
K1 O2 2.9234(16) . ?
K1 O4 2.7865(16) . ?
K1 O5 2.8523(9) 3_445 ?
K1 O5 2.8523(9) 7_566 ?
K1 O6 2.8899(9) 3_455 ?
K1 O6 2.8899(9) 7 ?
Zn1 K1 3.8518(5) 5_666 ?
Zn1 O2 2.1533(14) 5_666 ?
Zn1 O2 2.1533(14) . ?
Zn1 O4 2.1486(15) . ?
Zn1 O4 2.1486(15) 5_666 ?
Zn1 N1 2.1879(16) 5_666 ?
Zn1 N1 2.1879(16) . ?
C1 O1 1.2311(17) . ?
C1 N1 1.3633(15) . ?
C1 N3 1.3862(18) . ?
C2 O3 1.2425(17) . ?
C2 N2 1.3515(16) . ?
C2 N4 1.3792(19) . ?
C3 O5 1.222(2) . ?
C3 N3 1.3638(15) 2_656 ?
C3 N3 1.3637(15) . ?
C4 O6 1.222(2) . ?
C4 N4 1.3666(16) 2_655 ?
C4 N4 1.3666(16) . ?
O1 K1 2.8447(10) 5_666 ?
O2 H2 0.84(2) . ?
O4 H4 0.83(2) . ?
O5 K1 2.8524(9) 7_566 ?
O5 K1 2.8524(9) 3 ?
O6 K1 2.8899(9) 3_545 ?
O6 K1 2.8899(9) 7 ?
N1 C1 1.3633(15) 2_656 ?
N2 C2 1.3515(16) 2_655 ?
N3 H3 0.8600 . ?
N4 H4A 0.8600 . ?
