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#$Date: 2022-03-25 12:02:43 +0200 (Fri, 25 Mar 2022) $
#$Revision: 273990 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/48/8104875.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_8104875
loop_
_publ_author_name
'Oguntade, Bukunola K.'
'Hulushe, Siya T.'
'Hosten, Eric C.'
'Watkins, Gareth M.'
_publ_section_title
;
 Synthesis and crystal structure of hexaaquacopper(II)
 2,5-dicarboxyterephthalate, C10H16O14Cu
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              37
_journal_page_last               38
_journal_paper_doi               10.1515/ncrs-2020-0454
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C10 H4 O8, Cu H12 O6'
_chemical_formula_sum            'C10 H16 Cu O14'
_chemical_formula_weight         423.77
_chemical_name_systematic        'Hexaaquacopper(II) dihydrogen pyromellitate'
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.913(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2407(3)
_cell_length_b                   9.7565(4)
_cell_length_c                   21.1814(10)
_cell_measurement_reflns_used    4424
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.30
_cell_volume                     1492.85(11)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)[1]'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)[4]'
_computing_publication_material
'PLATON (Spek, 2009) [5], MERCURY (Macrae, 2008)[6], X-Seed (Barbour, 2001)[7]'
_computing_structure_refinement
'SHELXL-2018/3 (Sheldrick, 2015) and ShelXle (Hübschle, 2011)[3]'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)[2]'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6519
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.927
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8189
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.452
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1835
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0198
_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)+(0.0255P)²+1.1610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1729
_reflns_number_total             1835
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0454_suppl.cif
_cod_data_source_block           fa256
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               8104875
_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_min   0.522
_shelx_estimated_absorpt_t_max   0.752
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
Cu1 Cu 0.250000 0.29898(2) 0.500000 0.01188(7) Uani 1 2 d S T P . .
O1 O 0.65983(14) 0.62566(9) 0.27809(4) 0.0215(2) Uani 1 1 d . . . . .
H1 H 0.691389 0.614701 0.240993 0.026 Uiso 1 1 calc R U . . .
O2 O 0.55354(14) 0.49985(9) 0.35314(4) 0.0201(2) Uani 1 1 d . . . . .
O3 O 0.83469(15) 0.07623(10) 0.40118(4) 0.0230(2) Uani 1 1 d . . . . .
O4 O 0.78501(16) -0.09129(9) 0.33210(4) 0.0272(2) Uani 1 1 d . . . . .
O11 O 0.39511(15) 0.28873(10) 0.41953(4) 0.0214(2) Uani 1 1 d D . . . .
O12 O 0.250000 0.51463(14) 0.500000 0.0233(3) Uani 1 2 d DS T P . .
O13 O 0.250000 0.08946(14) 0.500000 0.0272(3) Uani 1 2 d DS T P . .
O14 O 0.50179(14) 0.31353(9) 0.55718(4) 0.01793(19) Uani 1 1 d D . . . .
C1 C 0.62713(17) 0.50851(12) 0.30253(6) 0.0148(2) Uani 1 1 d . . . . .
C2 C 0.68793(16) 0.37840(12) 0.27096(5) 0.0128(2) Uani 1 1 d . . . . .
C3 C 0.71930(17) 0.26832(13) 0.31202(6) 0.0137(2) Uani 1 1 d . . . . .
H3 H 0.697416 0.281195 0.355331 0.016 Uiso 1 1 calc R U . . .
C4 C 0.78085(16) 0.14049(12) 0.29336(5) 0.0131(2) Uani 1 1 d . . . . .
C5 C 0.80471(18) 0.03509(13) 0.34617(6) 0.0164(2) Uani 1 1 d . . . . .
H12 H 0.177(2) 0.5666(13) 0.5182(8) 0.038(5) Uiso 1 1 d D . . . .
H11A H 0.434(3) 0.3561(14) 0.4001(8) 0.042(6) Uiso 1 1 d D . . . .
H11B H 0.360(3) 0.2287(16) 0.3932(8) 0.050(6) Uiso 1 1 d D . . . .
H13 H 0.281(3) 0.0390(14) 0.4706(5) 0.046(6) Uiso 1 1 d D . . . .
H14A H 0.483(2) 0.3589(15) 0.5901(6) 0.030(5) Uiso 1 1 d D . . . .
H14B H 0.546(3) 0.2377(13) 0.5700(9) 0.046(6) Uiso 1 1 d 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'
Cu Cu 0.3201 1.2651 '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'
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
O13 Cu1 O11 87.22(3) . 2_556
O13 Cu1 O11 87.22(3) . .
O11 Cu1 O11 174.45(5) 2_556 .
O13 Cu1 O12 180.0 . .
O11 Cu1 O12 92.78(3) 2_556 .
O11 Cu1 O12 92.78(3) . .
O13 Cu1 O14 93.84(3) . 2_556
O11 Cu1 O14 90.49(4) 2_556 2_556
O11 Cu1 O14 89.88(4) . 2_556
O12 Cu1 O14 86.16(3) . 2_556
O13 Cu1 O14 93.84(3) . .
O11 Cu1 O14 89.88(4) 2_556 .
O11 Cu1 O14 90.49(4) . .
O12 Cu1 O14 86.16(3) . .
O14 Cu1 O14 172.33(5) 2_556 .
C1 O1 H1 109.5 . .
Cu1 O11 H11A 125.3(13) . .
Cu1 O11 H11B 115.8(15) . .
H11A O11 H11B 108.6(17) . .
Cu1 O12 H12 127.0(10) . .
Cu1 O12 H12 127.0(9) . 2_556
H12 O12 H12 106.0(19) . 2_556
Cu1 O13 H13 126.0(10) . .
Cu1 O13 H13 126.0(10) . 2_556
H13 O13 H13 108(2) . 2_556
Cu1 O14 H14A 109.0(12) . .
Cu1 O14 H14B 114.6(14) . .
H14A O14 H14B 105.9(15) . .
O2 C1 O1 120.97(11) . .
O2 C1 C2 118.87(11) . .
O1 C1 C2 120.09(11) . .
C3 C2 C4 118.27(11) . 7_655
C3 C2 C1 114.28(10) . .
C4 C2 C1 127.42(11) 7_655 .
C4 C3 C2 123.82(11) . .
C4 C3 H3 118.1 . .
C2 C3 H3 118.1 . .
C3 C4 C2 117.90(11) . 7_655
C3 C4 C5 114.83(10) . .
C2 C4 C5 127.27(11) 7_655 .
O3 C5 O4 122.93(11) . .
O3 C5 C4 118.50(11) . .
O4 C5 C4 118.50(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O13 2.0441(14) .
Cu1 O11 2.0648(9) 2_556
Cu1 O11 2.0648(9) .
Cu1 O12 2.1041(14) .
Cu1 O14 2.1235(10) 2_556
Cu1 O14 2.1236(10) .
O1 C1 1.2834(15) .
O1 H1 0.8400 .
O2 C1 1.2322(15) .
O3 C5 1.2375(15) .
O4 C5 1.2742(16) .
O11 H11A 0.836(9) .
O11 H11B 0.837(9) .
O12 H12 0.843(6) .
O12 H12 0.843(7) 2_556
O13 H13 0.837(7) .
O13 H13 0.837(7) 2_556
O14 H14A 0.845(9) .
O14 H14B 0.843(9) .
C1 C2 1.5141(16) .
C2 C3 1.3908(16) .
C2 C4 1.4082(16) 7_655
C3 C4 1.3907(17) .
C3 H3 0.9500 .
C4 C5 1.5206(16) .
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
O1 H1 O4 0.84 1.59 2.4181(13) 170 7_655 yes
O11 H11A O2 0.836(9) 1.954(10) 2.7851(13) 173(2) . yes
O11 H11B O4 0.837(9) 1.915(10) 2.7521(14) 179(2) 6 yes
O12 H12 O14 0.843(6) 1.951(7) 2.7936(13) 178(2) 6_565 yes
O13 H13 O3 0.837(7) 1.911(7) 2.7469(12) 176(2) 6 yes
O14 H14A O2 0.845(9) 1.859(10) 2.6811(12) 163.7(17) 5_666 yes
O14 H14B O3 0.843(9) 1.879(10) 2.7199(13) 175(2) 2_656 yes
C3 H3 O2 0.95 2.37 2.7285(15) 102 . yes
C3 H3 O3 0.95 2.41 2.7499(15) 101 . 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
O2 C1 C2 C3 -23.22(17) . . . .
O1 C1 C2 C3 153.68(12) . . . .
O2 C1 C2 C4 158.44(12) . . . 7_655
O1 C1 C2 C4 -24.66(19) . . . 7_655
C4 C2 C3 C4 0.4(2) 7_655 . . .
C1 C2 C3 C4 -178.14(11) . . . .
C2 C3 C4 C2 -0.4(2) . . . 7_655
C2 C3 C4 C5 -179.70(11) . . . .
C3 C4 C5 O3 -25.52(17) . . . .
C2 C4 C5 O3 155.22(13) 7_655 . . .
C3 C4 C5 O4 151.50(12) . . . .
C2 C4 C5 O4 -27.76(19) 7_655 . . .
