#------------------------------------------------------------------------------
#$Date: 2022-09-14 20:01:49 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/53/2215322.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_2215322
loop_
_publ_author_name
'Wang, Ming-Sheng'
'Zhou, Guo-Wei'
'Guo, Guo-Cong'
'Huang, Jin-Shun'
_publ_section_title
;
Poly[(μ₂-1,4-benzenedicarboxylato)aquadipyridinecopper(II)
0.25-hydrate]
;
_journal_coeditor_code           AT2383
_journal_issue                   10
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              m2524
_journal_page_last               m2524
_journal_paper_doi               10.1107/S1600536807043942
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (C8 H4 O4) (C5 H5 N)2 (H2 O)] , 0.25H2 O'
_chemical_formula_moiety         'C18 H16.50 Cu N2 O5.25'
_chemical_formula_sum            'C18 H16.5 Cu N2 O5.25'
_chemical_formula_weight         408.37
_chemical_name_systematic
;
Poly[(μ₂-1,4-benzenedicarboxylato)aquadipyridinecopper(II)
0.25-hydrate]
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9896(7)
_cell_length_b                   15.2593(18)
_cell_length_c                   21.581(2)
_cell_measurement_reflns_used    1986
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.31
_cell_volume                     1972.4(4)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995)'
_computing_structure_solution    'SHELXTL (Siemens, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0734
_diffrn_reflns_av_sigmaI/netI    0.1493
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5908
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             838
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .14
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.332
_refine_ls_abs_structure_details 'Flack (1983), 876 Friedel pairs'
_refine_ls_abs_structure_Flack   0.31(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2927
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                1689
_reflns_number_total             2927
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2383.cif
_cod_original_formula_sum        'C18 H16.50 Cu N2 O5.25'
_cod_database_code               2215322
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
Cu Cu1 0.16689(10) 0.53883(4) 0.34904(2) 0.03936(14) Uani d . 1
O O21 0.5303(6) 0.5146(3) 0.45248(14) 0.0864(16) Uani d . 1
O O22 0.1645(6) 0.49792(18) 0.43385(11) 0.0459(10) Uani d . 1
O O23 -0.0356(5) 0.4486(3) 0.74787(12) 0.0625(12) Uani d . 1
O O24 0.3310(6) 0.42383(19) 0.76355(11) 0.0486(10) Uani d . 1
C C21 0.1555(9) 0.4372(3) 0.72974(17) 0.0406(15) Uani d . 1
C C22 0.2054(7) 0.4467(3) 0.66137(15) 0.0368(14) Uani d . 1
C C23 0.4192(7) 0.4528(5) 0.63920(18) 0.068(2) Uani d . 1
H H23A 0.5386 0.4453 0.6662 0.082 Uiso calc R 1
C C24 0.4604(9) 0.4698(5) 0.5775(2) 0.090(2) Uani d . 1
H H24A 0.6068 0.4770 0.5640 0.107 Uiso calc R 1
C C25 0.2899(8) 0.4763(3) 0.53580(16) 0.0410(15) Uani d . 1
C C26 0.0789(7) 0.4670(4) 0.55662(18) 0.0547(17) Uani d . 1
H H26A -0.0401 0.4706 0.5291 0.066 Uiso calc R 1
C C27 0.0384(8) 0.4517(4) 0.62017(18) 0.0632(19) Uani d . 1
H H27A -0.1079 0.4449 0.6338 0.076 Uiso calc R 1
C C28 0.3415(11) 0.4975(3) 0.46790(19) 0.0523(17) Uani d . 1
N N11 0.1812(5) 0.41556(16) 0.31642(10) 0.0500(9) Uani d G 1
C C11 0.3632(5) 0.3621(2) 0.32926(15) 0.0810(16) Uani d G 1
H H11A 0.4814 0.3834 0.3528 0.097 Uiso calc R 1
C C12 0.3685(8) 0.2766(2) 0.3070(2) 0.103(2) Uani d G 1
H H12A 0.4903 0.2408 0.3156 0.124 Uiso calc R 1
C C13 0.1918(9) 0.24467(19) 0.27188(19) 0.111(2) Uani d G 1
H H13A 0.1953 0.1875 0.2570 0.133 Uiso calc R 1
C C14 0.0097(8) 0.2982(2) 0.25904(18) 0.128(2) Uani d G 1
H H14A -0.1085 0.2768 0.2355 0.154 Uiso calc R 1
C C15 0.0044(6) 0.3836(2) 0.28131(15) 0.0891(17) Uani d G 1
H H15A -0.1173 0.4194 0.2727 0.107 Uiso calc R 1
N N31 0.2070(5) 0.66163(17) 0.37881(11) 0.0500(9) Uani d G 1
C C31 0.3862(5) 0.7127(2) 0.35951(16) 0.0810(16) Uani d G 1
H H31A 0.4865 0.6908 0.3305 0.097 Uiso calc R 1
C C32 0.4155(7) 0.7964(2) 0.3836(2) 0.103(2) Uani d G 1
H H32A 0.5354 0.8305 0.3707 0.124 Uiso calc R 1
C C33 0.2655(9) 0.8290(2) 0.4270(2) 0.111(2) Uani d G 1
H H33A 0.2851 0.8850 0.4431 0.133 Uiso calc R 1
C C34 0.0863(8) 0.7780(2) 0.44630(18) 0.128(2) Uani d G 1
H H34A -0.0140 0.7999 0.4753 0.154 Uiso calc R 1
C C35 0.0571(6) 0.6943(2) 0.42221(15) 0.0891(17) Uani d G 1
H H35A -0.0628 0.6602 0.4351 0.107 Uiso calc R 1
O O1W -0.2068(4) 0.54786(18) 0.35159(9) 0.0553(10) Uani d D 1
H H1WA -0.2573(15) 0.5095(3) 0.37645(16) 0.083 Uiso d D 1
H H1WB -0.2802(11) 0.5393(6) 0.31842(15) 0.083 Uiso d D 1
O O2W 0.026(4) 0.2549(17) 0.4836(10) 0.178(5) Uani d PU 0.25
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'
Cu Cu 0.3201 1.2651 '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
O24 Cu1 O22 2_564 . 178.33(13)
O24 Cu1 N31 2_564 . 91.70(12)
O22 Cu1 N31 . . 89.96(11)
O24 Cu1 N11 2_564 . 86.63(11)
O22 Cu1 N11 . . 91.70(11)
N31 Cu1 N11 . . 170.51(13)
O24 Cu1 O1W 2_564 . 90.68(12)
O22 Cu1 O1W . . 89.38(12)
N31 Cu1 O1W . . 93.13(11)
N11 Cu1 O1W . . 96.23(12)
C28 O22 Cu1 . . 122.3(3)
C21 O24 Cu1 . 2_565 119.8(3)
O23 C21 O24 . . 127.0(4)
O23 C21 C22 . . 118.9(4)
O24 C21 C22 . . 113.8(4)
C27 C22 C23 . . 117.5(4)
C27 C22 C21 . . 120.3(4)
C23 C22 C21 . . 122.1(4)
C22 C23 C24 . . 121.2(4)
C22 C23 H23A . . 119.4
C24 C23 H23A . . 119.4
C25 C24 C23 . . 121.1(5)
C25 C24 H24A . . 119.5
C23 C24 H24A . . 119.5
C26 C25 C24 . . 118.3(4)
C26 C25 C28 . . 122.0(4)
C24 C25 C28 . . 119.7(4)
C25 C26 C27 . . 120.1(4)
C25 C26 H26A . . 119.9
C27 C26 H26A . . 119.9
C22 C27 C26 . . 121.7(4)
C22 C27 H27A . . 119.2
C26 C27 H27A . . 119.2
O21 C28 O22 . . 127.7(4)
O21 C28 C25 . . 119.9(5)
O22 C28 C25 . . 112.4(5)
C11 N11 C15 . . 120.0
C11 N11 Cu1 . . 120.88(15)
C15 N11 Cu1 . . 119.12(15)
C12 C11 N11 . . 120.0
C12 C11 H11A . . 120.0
N11 C11 H11A . . 120.0
C11 C12 C13 . . 120.0
C11 C12 H12A . . 120.0
C13 C12 H12A . . 120.0
C14 C13 C12 . . 120.0
C14 C13 H13A . . 120.0
C12 C13 H13A . . 120.0
C15 C14 C13 . . 120.0
C15 C14 H14A . . 120.0
C13 C14 H14A . . 120.0
C14 C15 N11 . . 120.0
C14 C15 H15A . . 120.0
N11 C15 H15A . . 120.0
C31 N31 C35 . . 120.0
C31 N31 Cu1 . . 121.51(15)
C35 N31 Cu1 . . 118.41(15)
C32 C31 N31 . . 120.0
C32 C31 H31A . . 120.0
N31 C31 H31A . . 120.0
C31 C32 C33 . . 120.0
C31 C32 H32A . . 120.0
C33 C32 H32A . . 120.0
C32 C33 C34 . . 120.0
C32 C33 H33A . . 120.0
C34 C33 H33A . . 120.0
C33 C34 C35 . . 120.0
C33 C34 H34A . . 120.0
C35 C34 H34A . . 120.0
C34 C35 N31 . . 120.0
C34 C35 H35A . . 120.0
N31 C35 H35A . . 120.0
Cu1 O1W H1WA . . 109.2(7)
Cu1 O1W H1WB . . 119.1(5)
H1WA O1W H1WB . . 103.9(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 O24 2_564 1.931(2)
Cu1 O22 . 1.934(2)
Cu1 N31 . 1.996(3)
Cu1 N11 . 2.010(3)
Cu1 O1W . 2.243(3)
O21 C28 . 1.208(7)
O22 C28 . 1.290(6)
O23 C21 . 1.222(6)
O24 C21 . 1.296(6)
O24 Cu1 2_565 1.931(2)
C21 C22 . 1.513(5)
C22 C27 . 1.341(6)
C22 C23 . 1.370(6)
C23 C24 . 1.380(6)
C23 H23A . 0.9300
C24 C25 . 1.364(6)
C24 H24A . 0.9300
C25 C26 . 1.349(6)
C25 C28 . 1.532(6)
C26 C27 . 1.412(6)
C26 H26A . 0.9300
C27 H27A . 0.9300
N11 C11 . 1.3900
N11 C15 . 1.3900
C11 C12 . 1.3900
C11 H11A . 0.9300
C12 C13 . 1.3900
C12 H12A . 0.9300
C13 C14 . 1.3900
C13 H13A . 0.9300
C14 C15 . 1.3900
C14 H14A . 0.9300
C15 H15A . 0.9300
N31 C31 . 1.3900
N31 C35 . 1.3900
C31 C32 . 1.3900
C31 H31A . 0.9300
C32 C33 . 1.3900
C32 H32A . 0.9300
C33 C34 . 1.3900
C33 H33A . 0.9300
C34 C35 . 1.3900
C34 H34A . 0.9300
C35 H35A . 0.9300
O1W H1WA . 0.850(4)
O1W H1WB . 0.850(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
O1W H1WA O21 1_455 0.850(4) 2.078(7) 2.735(4) 133.7(6) y
O1W H1WB O23 2_464 0.850(4) 1.889(5) 2.719(3) 164.9(10) y
