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#$Date: 2021-02-24 12:01:25 +0200 (Wed, 24 Feb 2021) $
#$Revision: 262189 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/06/1560608.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_1560608
loop_
_publ_author_name
'Xu, Qing-Qing'
'Liu, Bing'
'Xu, Ling'
'Jiao, Huan'
_publ_section_title
;
 Ionothermal synthesis and structural transformation targeted by ion
 exchange in metal-1,3,5-benzenetricarboxylate compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               7
_journal_paper_doi               10.1016/j.jssc.2016.12.006
_journal_volume                  247
_journal_year                    2017
_chemical_formula_moiety         '0.5(C18 H22 Cl2 Cu4 O20)'
_chemical_formula_sum            'C9 H11 Cl Cu2 O10'
_chemical_formula_weight         441.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3641(11)
_cell_length_b                   14.1462(11)
_cell_length_c                   7.4643(6)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.88
_cell_volume                     1516.7(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_molecular_graphics    'Siemens SHELXTLTM 5'
_computing_publication_material  'Siemens SHELXTLTM 5'
_computing_structure_refinement  'Siemens SHELXTLTM 5'
_computing_structure_solution    'Siemens SHELXTLTM 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18093
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'rotating-anode generator'
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (CrystalClear)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0299
_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)+(0.0511P)²+4.8854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                688
_reflns_number_total             746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mmc7.CIF
_cod_data_source_block           comp3
_cod_database_code               1560608
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 Cu1, O1W
 with sigma for 1-2 distances of 0.4 and sigma for 1-3 distances of 0.2
3.a Rotating group:
 O1W(H1Wa,H1Wb)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, -z+1/2'
4 'x, -y, -z'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 '-x+1/2, y+1/2, -z+1/2'
8 'x+1/2, -y+1/2, -z'
9 '-x, -y, -z'
10 'x, y, -z-1/2'
11 'x, -y, z-1/2'
12 '-x, y, z'
13 '-x+1/2, -y+1/2, -z'
14 'x+1/2, y+1/2, -z-1/2'
15 'x+1/2, -y+1/2, z-1/2'
16 '-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.64298(3) 0.13362(3) 0.7500 0.0248(2) Uani 1 2 d SU . .
Cl1 Cl 0.5000 0.00967(9) 0.7500 0.0247(3) Uani 1 4 d S . .
O12 O 0.74859(18) 0.54685(19) 0.7500 0.0303(7) Uani 1 2 d S . .
O13 O 0.6774(2) 0.68585(19) 0.7500 0.0369(8) Uani 1 2 d S . .
O11 O 0.5761(2) 0.2542(2) 0.7500 0.0671(14) Uani 1 2 d S . .
O1W O 0.64675(19) 0.13533(16) 0.4823(4) 0.0544(8) Uani 1 1 d U . .
H1WA H 0.5975 0.1080 0.4373 0.082 Uiso 1 1 d R . .
H1WB H 0.6958 0.1056 0.4423 0.082 Uiso 1 1 d R . .
C13 C 0.5843(2) 0.5462(3) 0.7500 0.0203(8) Uani 1 2 d S . .
C14 C 0.5000 0.5952(4) 0.7500 0.0224(12) Uani 1 4 d S . .
H14 H 0.5000 0.6609 0.7500 0.027 Uiso 1 4 calc SR . .
C11 C 0.5000 0.3989(4) 0.7500 0.0192(11) Uani 1 4 d S . .
C16 C 0.6753(3) 0.5981(3) 0.7500 0.0249(9) Uani 1 2 d S . .
C15 C 0.5000 0.2926(4) 0.7500 0.0236(12) Uani 1 4 d S . .
C12 C 0.5835(3) 0.4477(3) 0.7500 0.0225(8) Uani 1 2 d S . .
H12 H 0.6394 0.4146 0.7500 0.027 Uiso 1 2 calc SR . .
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'
Cl Cl 0.1484 0.1585 '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
O12 Cu1 Cl1 101.27(8) 7_646 .
O12 Cu1 O1W 89.21(8) 7_646 10_557
O12 Cu1 O1W 89.21(8) 7_646 .
O11 Cu1 Cl1 101.10(11) . .
O11 Cu1 O12 157.62(13) . 7_646
O11 Cu1 O1W 90.16(7) . .
O11 Cu1 O1W 90.16(7) . 10_557
O1W Cu1 Cl1 91.63(7) 10_557 .
O1W Cu1 Cl1 91.63(7) . .
O1W Cu1 O1W 176.60(16) . 10_557
Cu1 Cl1 Cu1 99.02(5) . 3_656
C16 O12 Cu1 107.2(2) . 7_656
C15 O11 Cu1 145.8(3) . .
Cu1 O1W H1WA 110.9 . .
Cu1 O1W H1WB 111.0 . .
H1WA O1W H1WB 108.0 . .
C14 C13 C16 120.9(3) . .
C12 C13 C14 119.3(3) . .
C12 C13 C16 119.8(3) . .
C13 C14 C13 120.5(5) 3_656 .
C13 C14 H14 119.8 3_656 .
C13 C14 H14 119.8 . .
C12 C11 C15 120.0(2) 3_656 .
C12 C11 C15 120.0(2) . .
C12 C11 C12 120.1(5) . 3_656
O12 C16 C13 116.2(3) . .
O13 C16 O12 123.2(3) . .
O13 C16 C13 120.6(3) . .
O11 C15 O11 127.1(5) 3_656 .
O11 C15 C11 116.4(3) 3_656 .
O11 C15 C11 116.4(3) . .
C13 C12 H12 119.8 . .
C11 C12 C13 120.4(4) . .
C11 C12 H12 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl1 2.7004(10) .
Cu1 O12 1.983(3) 7_646
Cu1 O11 1.958(3) .
Cu1 O1W 1.999(3) 10_557
Cu1 O1W 1.999(3) .
Cl1 Cu1 2.7004(10) 3_656
O12 Cu1 1.983(3) 7_656
O12 C16 1.278(5) .
O13 C16 1.242(5) .
O11 C15 1.221(4) .
O1W H1WA 0.8736 .
O1W H1WB 0.8734 .
C13 C14 1.395(4) .
C13 C16 1.499(5) .
C13 C12 1.394(5) .
C14 C13 1.395(4) 3_656
C14 H14 0.9300 .
C11 C15 1.503(7) .
C11 C12 1.384(4) 3_656
C11 C12 1.384(4) .
C15 O11 1.221(4) 3_656
C12 H12 0.9300 .
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
Cu1 O12 C16 O13 0.0 7_656 . . .
Cu1 O12 C16 C13 180.0 7_656 . . .
Cu1 O11 C15 O11 0.0 . . . 3_656
Cu1 O11 C15 C11 180.0 . . . .
Cl1 Cu1 O11 C15 0.0 . . . .
O12 Cu1 Cl1 Cu1 180.0 7_646 . . 3_656
O12 Cu1 O11 C15 180.0 7_646 . . .
O11 Cu1 Cl1 Cu1 0.0 . . . 3_656
O1W Cu1 Cl1 Cu1 -90.48(8) . . . 3_656
O1W Cu1 Cl1 Cu1 90.48(8) 10_557 . . 3_656
O1W Cu1 O11 C15 -91.70(8) 10_557 . . .
O1W Cu1 O11 C15 91.70(8) . . . .
C14 C13 C16 O12 180.0 . . . .
C14 C13 C16 O13 0.0 . . . .
C14 C13 C12 C11 0.0 . . . .
C16 C13 C14 C13 180.0 . . . 3_656
C16 C13 C12 C11 180.0 . . . .
C15 C11 C12 C13 180.0 . . . .
C12 C13 C14 C13 0.0 . . . 3_656
C12 C13 C16 O12 0.0 . . . .
C12 C13 C16 O13 180.0 . . . .
C12 C11 C15 O11 180.0 3_656 . . .
C12 C11 C15 O11 0.0 3_656 . . 3_656
C12 C11 C15 O11 0.0 . . . .
C12 C11 C15 O11 180.0 . . . 3_656
C12 C11 C12 C13 0.0 3_656 . . .
