#------------------------------------------------------------------------------
#$Date: 2025-08-19 16:18:28 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/22/66/2226604.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2226604
loop_
_publ_author_name
'Nie, Jing-Jing'
'Pan, Tian-Tian'
'Su, Jian-Rong'
'Xu, Duan-Jun'
_publ_section_title
;
 Bis(μ-2,4-dihydroxybenzoato-κ²O:O')bis[aqua(2,4-dihydroxybenzoato-κO)(1,10-phenanthroline-κ²N,N')cadmium(II)]
;
_journal_coeditor_code           NG2775
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m760
_journal_page_last               m761
_journal_paper_doi               10.1107/S1600536810021252
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cd2 (C7 H5 O4)4 (C12 H8 N2)2 (H2 O1)2]'
_chemical_formula_moiety         'C52 H40 Cd2 N4 O18'
_chemical_formula_sum            'C52 H40 Cd2 N4 O18'
_chemical_formula_weight         1233.68
_chemical_name_systematic
;
Bis(μ-2,4-dihydroxybenzoato-κ²O:O')bis[aqua(2,4-
dihydroxybenzoato-κO)(1,10-phenanthroline-
κ²N,N')cadmium(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.378(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.899(4)
_cell_length_b                   6.874(2)
_cell_length_c                   23.400(6)
_cell_measurement_reflns_used    15860
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.1
_cell_volume                     2331.5(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19273
_diffrn_reflns_theta_full        26.14
_diffrn_reflns_theta_max         26.1
_diffrn_reflns_theta_min         3.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.379
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0281P)²+1.5199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                4015
_reflns_number_total             4654
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2775.cif
_cod_data_source_block           I
_cod_original_cell_volume        2331.4(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2226604
_cod_database_fobs_code          2226604
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.397190(12) 0.67327(3) 0.425111(8) 0.03048(7) Uani d . 1 . .
N N1 0.37208(16) 0.6779(3) 0.32325(9) 0.0369(5) Uani d . 1 . .
N N2 0.53505(15) 0.7623(3) 0.40192(9) 0.0329(5) Uani d . 1 . .
O O1 0.25877(13) 0.5555(3) 0.42507(10) 0.0534(6) Uani d . 1 . .
O O2 0.16636(15) 0.8085(3) 0.39648(12) 0.0592(6) Uani d . 1 . .
O O3 -0.00646(15) 0.7698(3) 0.38480(10) 0.0421(5) Uani d P 0.90 A 1
H H3A 0.0419 0.8218 0.3821 0.063 Uiso calc PR 0.90 A 1
O O3' 0.2006(13) 0.254(3) 0.4445(9) 0.040(4) Uani d P 0.10 A 2
H H3B 0.2343 0.3426 0.4388 0.060 Uiso calc PR 0.10 A 2
O O4 -0.11493(14) 0.1736(3) 0.44782(11) 0.0531(5) Uani d . 1 A .
H H4A -0.1643 0.2313 0.4387 0.080 Uiso calc R 1 . .
O O5 0.44142(12) 0.3360(3) 0.43181(8) 0.0376(4) Uani d . 1 . .
O O6 0.58823(14) 0.2947(3) 0.47871(8) 0.0465(5) Uani d . 1 . .
O O7 0.71417(12) 0.3368(3) 0.42386(8) 0.0453(5) Uani d . 1 . .
H H7A 0.6910 0.3342 0.4524 0.068 Uiso calc R 1 . .
O O8 0.63878(16) 0.2938(4) 0.21875(9) 0.0554(6) Uani d . 1 . .
H H8A 0.5953 0.2774 0.1905 0.083 Uiso calc R 1 . .
O O9 0.33412(15) 0.9899(3) 0.41432(12) 0.0584(6) Uani d D 1 . .
H H9A 0.2763(6) 0.977(6) 0.4129(16) 0.070 Uiso d D 1 . .
H H9B 0.353(3) 1.1085(18) 0.4142(16) 0.070 Uiso d D 1 . .
C C1 0.18095(18) 0.6359(5) 0.41415(12) 0.0408(7) Uani d . 1 . .
C C2 0.10138(17) 0.5164(4) 0.42243(10) 0.0324(5) Uani d . 1 A .
C C3 0.01181(18) 0.5888(4) 0.40876(11) 0.0330(6) Uani d . 1 . .
H H3 0.0011 0.7142 0.3939 0.040 Uiso calc PR 0.10 A 2
C C4 -0.06174(17) 0.4778(4) 0.41683(11) 0.0350(6) Uani d . 1 A .
H H4 -0.1212 0.5289 0.4077 0.042 Uiso calc R 1 . .
C C5 -0.04658(18) 0.2906(4) 0.43854(12) 0.0349(6) Uani d . 1 . .
C C6 0.04272(16) 0.2132(4) 0.45253(13) 0.0386(6) Uani d D 1 A .
H H6 0.0532 0.0874 0.4672 0.046 Uiso calc R 1 . .
C C7 0.11485(15) 0.3269(4) 0.44412(11) 0.0366(6) Uani d D 1 . .
H H7 0.1742 0.2758 0.4532 0.044 Uiso calc PR 0.90 A 1
C C8 0.52452(18) 0.3071(4) 0.43170(11) 0.0314(5) Uani d . 1 . .
C C9 0.55409(17) 0.2915(3) 0.37581(11) 0.0295(5) Uani d . 1 . .
C C10 0.64719(18) 0.3133(4) 0.37392(11) 0.0338(5) Uani d . 1 . .
C C11 0.67359(19) 0.3138(4) 0.32113(12) 0.0412(6) Uani d . 1 . .
H H11 0.7354 0.3295 0.3206 0.049 Uiso calc R 1 . .
C C12 0.6079(2) 0.2908(4) 0.26885(12) 0.0384(6) Uani d . 1 . .
C C13 0.5157(2) 0.2642(4) 0.26956(12) 0.0378(6) Uani d . 1 . .
H H13 0.4717 0.2452 0.2347 0.045 Uiso calc R 1 . .
C C14 0.49017(18) 0.2662(4) 0.32251(12) 0.0343(6) Uani d . 1 . .
H H14 0.4283 0.2501 0.3227 0.041 Uiso calc R 1 . .
C C15 0.2934(2) 0.6307(5) 0.28578(13) 0.0469(7) Uani d . 1 . .
H H15 0.2427 0.5985 0.3007 0.056 Uiso calc R 1 . .
C C16 0.2839(3) 0.6274(5) 0.22552(14) 0.0568(9) Uani d . 1 . .
H H16 0.2281 0.5924 0.2006 0.068 Uiso calc R 1 . .
C C17 0.3582(3) 0.6768(5) 0.20315(13) 0.0541(8) Uani d . 1 . .
H H17 0.3529 0.6768 0.1628 0.065 Uiso calc R 1 . .
C C18 0.4424(2) 0.7273(4) 0.24132(12) 0.0425(7) Uani d . 1 . .
C C19 0.5236(3) 0.7702(5) 0.22142(14) 0.0523(8) Uani d . 1 . .
H H19 0.5212 0.7717 0.1813 0.063 Uiso calc R 1 . .
C C20 0.6036(3) 0.8083(5) 0.25983(15) 0.0525(8) Uani d . 1 . .
H H20 0.6557 0.8362 0.2458 0.063 Uiso calc R 1 . .
C C21 0.6106(2) 0.8070(4) 0.32217(13) 0.0404(6) Uani d . 1 . .
C C22 0.6939(2) 0.8440(5) 0.36345(15) 0.0512(8) Uani d . 1 . .
H H22 0.7474 0.8713 0.3509 0.061 Uiso calc R 1 . .
C C23 0.6955(2) 0.8396(5) 0.42162(15) 0.0502(8) Uani d . 1 . .
H H23 0.7498 0.8653 0.4493 0.060 Uiso calc R 1 . .
C C24 0.6148(2) 0.7962(4) 0.43937(13) 0.0420(7) Uani d . 1 . .
H H24 0.6170 0.7908 0.4794 0.050 Uiso calc R 1 . .
C C25 0.53247(19) 0.7677(4) 0.34348(11) 0.0325(6) Uani d . 1 . .
C C26 0.4460(2) 0.7251(4) 0.30205(11) 0.0337(6) Uani 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cd O6 . 3_666 84.81(8) ?
O1 Cd N2 . . 165.66(8) ?
O6 Cd N2 3_666 . 109.02(8) ?
O1 Cd N1 . . 94.34(8) ?
O6 Cd N1 3_666 . 172.63(8) ?
N2 Cd N1 . . 72.45(8) ?
O1 Cd O9 . . 89.40(8) ?
O6 Cd O9 3_666 . 87.72(9) ?
N2 Cd O9 . . 94.81(8) ?
N1 Cd O9 . . 84.96(9) ?
O1 Cd O5 . . 83.61(8) ?
O6 Cd O5 3_666 . 93.93(7) ?
N2 Cd O5 . . 91.45(7) ?
N1 Cd O5 . . 93.25(7) ?
O9 Cd O5 . . 172.64(7) ?
C15 N1 C26 . . 119.1(2) ?
C15 N1 Cd . . 125.4(2) ?
C26 N1 Cd . . 115.42(17) ?
C24 N2 C25 . . 118.2(2) ?
C24 N2 Cd . . 126.73(18) ?
C25 N2 Cd . . 114.91(17) ?
C1 O1 Cd . . 130.9(2) ?
C3 O3 H3A . . 109.5 ?
C7 O3' H3B . . 109.5 ?
C5 O4 H4A . . 109.5 ?
C8 O5 Cd . . 114.07(16) ?
C8 O6 Cd . 3_666 138.08(18) ?
C10 O7 H7A . . 109.5 ?
C12 O8 H8A . . 109.5 ?
Cd O9 H9A . . 106(3) ?
Cd O9 H9B . . 139(3) ?
H9A O9 H9B . . 115(4) ?
O1 C1 O2 . . 124.3(3) ?
O1 C1 C2 . . 117.0(3) ?
O2 C1 C2 . . 118.7(3) ?
C3 C2 C7 . . 117.9(2) ?
C3 C2 C1 . . 121.5(3) ?
C7 C2 C1 . . 120.7(2) ?
O3 C3 C4 . . 118.0(2) ?
O3 C3 C2 . . 120.7(2) ?
C4 C3 C2 . . 121.3(2) ?
C4 C3 H3 . . 119.3 ?
C2 C3 H3 . . 119.3 ?
C5 C4 C3 . . 119.7(2) ?
C5 C4 H4 . . 120.1 ?
C3 C4 H4 . . 120.1 ?
O4 C5 C4 . . 123.1(2) ?
O4 C5 C6 . . 116.5(2) ?
C4 C5 C6 . . 120.4(2) ?
C7 C6 C5 . . 118.7(2) ?
C7 C6 H6 . . 120.6 ?
C5 C6 H6 . . 120.6 ?
O3' C7 C6 . . 123.2(8) ?
O3' C7 C2 . . 113.5(8) ?
C6 C7 C2 . . 122.0(2) ?
C6 C7 H7 . . 119.0 ?
C2 C7 H7 . . 119.0 ?
O5 C8 O6 . . 123.0(2) ?
O5 C8 C9 . . 120.7(2) ?
O6 C8 C9 . . 116.3(2) ?
C14 C9 C10 . . 117.4(2) ?
C14 C9 C8 . . 121.3(2) ?
C10 C9 C8 . . 121.2(2) ?
O7 C10 C11 . . 117.7(2) ?
O7 C10 C9 . . 121.3(2) ?
C11 C10 C9 . . 121.1(2) ?
C10 C11 C12 . . 120.0(3) ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
O8 C12 C11 . . 116.7(3) ?
O8 C12 C13 . . 123.1(3) ?
C11 C12 C13 . . 120.1(2) ?
C14 C13 C12 . . 119.2(2) ?
C14 C13 H13 . . 120.4 ?
C12 C13 H13 . . 120.4 ?
C13 C14 C9 . . 122.2(2) ?
C13 C14 H14 . . 118.9 ?
C9 C14 H14 . . 118.9 ?
N1 C15 C16 . . 122.8(3) ?
N1 C15 H15 . . 118.6 ?
C16 C15 H15 . . 118.6 ?
C17 C16 C15 . . 118.9(3) ?
C17 C16 H16 . . 120.6 ?
C15 C16 H16 . . 120.6 ?
C16 C17 C18 . . 119.9(3) ?
C16 C17 H17 . . 120.0 ?
C18 C17 H17 . . 120.0 ?
C17 C18 C26 . . 117.3(3) ?
C17 C18 C19 . . 123.0(3) ?
C26 C18 C19 . . 119.6(3) ?
C20 C19 C18 . . 120.8(3) ?
C20 C19 H19 . . 119.6 ?
C18 C19 H19 . . 119.6 ?
C19 C20 C21 . . 121.5(3) ?
C19 C20 H20 . . 119.2 ?
C21 C20 H20 . . 119.2 ?
C25 C21 C22 . . 117.7(3) ?
C25 C21 C20 . . 119.5(3) ?
C22 C21 C20 . . 122.7(3) ?
C23 C22 C21 . . 119.5(3) ?
C23 C22 H22 . . 120.2 ?
C21 C22 H22 . . 120.2 ?
C22 C23 C24 . . 119.2(3) ?
C22 C23 H23 . . 120.4 ?
C24 C23 H23 . . 120.4 ?
N2 C24 C23 . . 123.0(3) ?
N2 C24 H24 . . 118.5 ?
C23 C24 H24 . . 118.5 ?
N2 C25 C21 . . 122.2(3) ?
N2 C25 C26 . . 118.7(2) ?
C21 C25 C26 . . 119.1(2) ?
N1 C26 C18 . . 122.0(3) ?
N1 C26 C25 . . 118.5(2) ?
C18 C26 C25 . . 119.5(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cd N1 . 2.326(2) y
Cd N2 . 2.324(2) y
Cd O1 . 2.215(2) y
Cd O5 . 2.406(2) y
Cd O6 3_666 2.2215(19) y
Cd O9 . 2.361(2) y
N1 C15 . 1.331(4) ?
N1 C26 . 1.348(4) ?
N2 C24 . 1.324(3) ?
N2 C25 . 1.360(3) ?
O1 C1 . 1.256(3) ?
O2 C1 . 1.258(4) ?
O3 C3 . 1.366(3) ?
O3 H3A . 0.8200 ?
O3' C7 . 1.370(18) ?
O3' H3B . 0.8200 ?
O4 C5 . 1.354(3) ?
O4 H4A . 0.8200 ?
O5 C8 . 1.254(3) ?
O6 C8 . 1.279(3) ?
O6 Cd 3_666 2.222(2) ?
O7 C10 . 1.359(3) ?
O7 H7A . 0.8200 ?
O8 C12 . 1.355(3) ?
O8 H8A . 0.8200 ?
O9 H9A . 0.860(11) ?
O9 H9B . 0.862(14) ?
C1 C2 . 1.491(4) ?
C2 C3 . 1.390(4) ?
C2 C7 . 1.395(4) ?
C3 C4 . 1.384(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.382(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.400(4) ?
C6 C7 . 1.379(4) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 C9 . 1.477(3) ?
C9 C14 . 1.394(4) ?
C9 C10 . 1.406(4) ?
C10 C11 . 1.380(4) ?
C11 C12 . 1.388(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.390(4) ?
C13 C14 . 1.378(4) ?
C13 H13 . 0.9300 ?
C14 H14 . 0.9300 ?
C15 C16 . 1.384(4) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.373(5) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.404(5) ?
C17 H17 . 0.9300 ?
C18 C26 . 1.410(4) ?
C18 C19 . 1.425(5) ?
C19 C20 . 1.342(5) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.438(4) ?
C20 H20 . 0.9300 ?
C21 C25 . 1.395(4) ?
C21 C22 . 1.407(4) ?
C22 C23 . 1.356(5) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.392(4) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
C25 C26 . 1.452(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O3 H3A O2 . 0.82 1.81 2.540(3) 148 y
O3' H3B O1 . 0.82 1.56 2.332(19) 156 y
O4 H4A O7 1_455 0.82 1.91 2.719(3) 172 y
O7 H7A O6 . 0.82 1.80 2.523(3) 147 y
O8 H8A O3 2_545 0.82 1.94 2.752(3) 169 y
O9 H9A O2 . 0.860(11) 1.969(19) 2.738(3) 148(3) y
O9 H9B O5 1_565 0.862(14) 2.03(2) 2.842(3) 158(3) y
C24 H24 O5 3_666 0.93 2.58 3.433(4) 152 y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168309860
