#------------------------------------------------------------------------------
#$Date: 2023-06-13 10:41:25 +0300 (Tue, 13 Jun 2023) $
#$Revision: 284456 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/73/8107352.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_8107352
loop_
_publ_author_name
'Huang, Yujiao'
'Li, Ben'
'Miao, Siyi'
'Luo, Linhui'
'Pang, Haixia'
'Tang, Qiang'
_publ_section_title
;
 Crystal structure of diaqua-bis(4-(hydroxymethyl)-benzoato-k1 O)zinc(II),
 C16H18O8Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              57
_journal_page_last               59
_journal_paper_doi               10.1515/ncrs-2022-0428
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C16 H18 O8 Zn'
_chemical_formula_sum            'C16 H18 O8 Zn'
_chemical_formula_weight         403.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.536(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.152(2)
_cell_length_b                   5.0051(8)
_cell_length_c                   27.273(5)
_cell_measurement_reflns_used    1467
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      22.65
_cell_measurement_theta_min      3.05
_cell_volume                     1625.3(5)
_computing_cell_refinement       'Bruker SAINT(Bruker, 2009)'
_computing_data_collection       'Bruker APEX2[1]'
_computing_data_reduction        'Bruker SAINT(Bruker, 2009)'
_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)[2]'
_computing_structure_solution    'XM  (Sheldrick, 2008)[3]'
_diffrn_ambient_temperature      296(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            8502
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.161
_diffrn_reflns_theta_min         3.049
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick,2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0516
_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/[σ²(Fo²)+(0.0753P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1804
_reflns_number_total             2683
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0428_suppl.cif
_cod_data_source_block           mo
_cod_database_code               8107352
_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.
;
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O3(H3A,H3B), O4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.250000 0.07395(9) 0.500000 0.03397(17) Uani 1 2 d S T P . .
O1 O 0.23136(17) 0.3320(4) 0.44306(7) 0.0356(4) Uani 1 1 d . . . . .
O2 O 0.41157(18) 0.2527(4) 0.46461(8) 0.0418(5) Uani 1 1 d . . . . .
O3 O 0.36122(17) -0.2058(4) 0.52767(8) 0.0422(5) Uani 1 1 d . . . . .
H3A H 0.335282 -0.306215 0.546251 0.063 Uiso 1 1 d R U . . .
H3B H 0.418732 -0.135805 0.543211 0.063 Uiso 1 1 d R U . . .
O4 O 0.4828(3) 1.1050(5) 0.26783(13) 0.0858(12) Uani 1 1 d . . . . .
H4 H 0.467313 0.955961 0.255949 0.129 Uiso 1 1 d R U . . .
C1 C 0.3498(2) 0.5713(5) 0.39939(10) 0.0284(5) Uani 1 1 d . . . . .
C2 C 0.4550(3) 0.6760(7) 0.40037(11) 0.0393(7) Uani 1 1 d . . . . .
H2 H 0.515386 0.620562 0.424821 0.047 Uiso 1 1 calc R U . . .
C3 C 0.4715(3) 0.8643(7) 0.36501(12) 0.0423(7) Uani 1 1 d . . . . .
H3 H 0.542939 0.933144 0.365899 0.051 Uiso 1 1 calc R U . . .
C4 C 0.3826(3) 0.9498(6) 0.32860(11) 0.0396(7) Uani 1 1 d . . . . .
C5 C 0.2783(3) 0.8448(8) 0.32810(12) 0.0478(8) Uani 1 1 d . . . . .
H5 H 0.217923 0.901357 0.303734 0.057 Uiso 1 1 calc R U . . .
C6 C 0.2604(2) 0.6582(7) 0.36264(11) 0.0404(7) Uani 1 1 d . . . . .
H6 H 0.188711 0.590100 0.361469 0.049 Uiso 1 1 calc R U . . .
C7 C 0.3326(2) 0.3712(5) 0.43759(10) 0.0308(6) Uani 1 1 d . . . . .
C8 C 0.3997(4) 1.1633(8) 0.29231(15) 0.0607(11) Uani 1 1 d . . . . .
H8A H 0.330318 1.188505 0.268086 0.073 Uiso 1 1 calc R U . . .
H8B H 0.417269 1.330152 0.310276 0.073 Uiso 1 1 calc R U . . .
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'
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
O1 Zn1 O1 99.45(12) 2_556 .
O3 Zn1 O1 135.52(8) . .
O3 Zn1 O1 101.39(9) . 2_556
O3 Zn1 O1 135.53(8) 2_556 2_556
O3 Zn1 O1 101.39(9) 2_556 .
O3 Zn1 O3 90.40(13) . 2_556
C7 O1 Zn1 103.12(18) . .
Zn1 O3 H3A 110.5 . .
Zn1 O3 H3B 109.9 . .
H3A O3 H3B 109.6 . .
C8 O4 H4 104.9 . .
C2 C1 C6 118.9(3) . .
C2 C1 C7 120.1(2) . .
C6 C1 C7 121.0(2) . .
C1 C2 H2 119.8 . .
C1 C2 C3 120.4(3) . .
C3 C2 H2 119.8 . .
C2 C3 H3 119.7 . .
C4 C3 C2 120.5(3) . .
C4 C3 H3 119.7 . .
C3 C4 C8 120.2(3) . .
C5 C4 C3 118.5(3) . .
C5 C4 C8 121.2(3) . .
C4 C5 H5 119.1 . .
C4 C5 C6 121.8(3) . .
C6 C5 H5 119.1 . .
C1 C6 H6 120.1 . .
C5 C6 C1 119.9(3) . .
C5 C6 H6 120.1 . .
O1 C7 C1 117.1(2) . .
O2 C7 O1 120.3(2) . .
O2 C7 C1 122.5(3) . .
O4 C8 C4 112.9(3) . .
O4 C8 H8A 109.0 . .
O4 C8 H8B 109.0 . .
C4 C8 H8A 109.0 . .
C4 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.997(2) .
Zn1 O1 1.997(2) 2_556
Zn1 O3 1.987(2) 2_556
Zn1 O3 1.987(2) .
O1 C7 1.283(3) .
O2 C7 1.238(3) .
O3 H3A 0.8200 .
O3 H3B 0.8200 .
O4 H4 0.8200 .
O4 C8 1.349(4) .
C1 C2 1.377(4) .
C1 C6 1.392(4) .
C1 C7 1.490(4) .
C2 H2 0.9300 .
C2 C3 1.391(4) .
C3 H3 0.9300 .
C3 C4 1.381(5) .
C4 C5 1.370(5) .
C4 C8 1.499(4) .
C5 H5 0.9300 .
C5 C6 1.374(5) .
C6 H6 0.9300 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3A O1 0.82 2.03 2.759(3) 148.2 2_546 yes
O3 H3B O2 0.82 2.19 2.737(3) 123.8 5_656 yes
O4 H4 O4 0.82 2.01 2.747(2) 149.7 4_545 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Zn1 O1 C7 O2 1.2(3) . . . .
Zn1 O1 C7 C1 -176.22(19) . . . .
C1 C2 C3 C4 0.3(5) . . . .
C2 C1 C6 C5 0.2(5) . . . .
C2 C1 C7 O1 162.6(3) . . . .
C2 C1 C7 O2 -14.7(4) . . . .
C2 C3 C4 C5 -0.1(5) . . . .
C2 C3 C4 C8 176.7(3) . . . .
C3 C4 C5 C6 -0.1(5) . . . .
C3 C4 C8 O4 54.5(5) . . . .
C4 C5 C6 C1 0.0(5) . . . .
C5 C4 C8 O4 -128.7(4) . . . .
C6 C1 C2 C3 -0.4(5) . . . .
C6 C1 C7 O1 -16.5(4) . . . .
C6 C1 C7 O2 166.1(3) . . . .
C7 C1 C2 C3 -179.6(3) . . . .
C7 C1 C6 C5 179.4(3) . . . .
C8 C4 C5 C6 -176.9(3) . . . .
