#------------------------------------------------------------------------------
#$Date: 2019-10-12 03:39:55 +0300 (Sat, 12 Oct 2019) $
#$Revision: 219305 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234570.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_7234570
loop_
_publ_author_name
'Zhang, Jun'
'Ma, Xiaofan'
'Kong, Weili'
'Lu, Guodong'
'Xuan, Xiaopeng'
_publ_section_title
;
 Cooperative proton transportation based on the reversible single
 crystal--single crystal transformation in a highly water-stable Cu-MOF
 with its facile and scalable preparation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01334B
_journal_year                    2019
_chemical_formula_moiety         '0.5(C20 H4 Cu4 O18), H6 O2'
_chemical_formula_sum            'C10 H8 Cu2 O11'
_chemical_formula_weight         431.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-10 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.552(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8682(3)
_cell_length_b                   10.5629(4)
_cell_length_c                   11.6070(5)
_cell_measurement_reflns_used    1707
_cell_measurement_temperature    298.3(1)
_cell_measurement_theta_max      70.3340
_cell_measurement_theta_min      4.2100
_cell_volume                     924.70(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.3(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00 -19.00   0.50    0.05    --   -2.46  57.00 150.00   62
  2  ω      3.00  29.00   0.50    0.05    --   -2.46  57.00 150.00   52
  3  ω     54.00  80.00   0.50    0.05    --   -2.46  57.00 150.00   52
  4  ω      0.00  41.00   0.50    0.05    --   -2.46 -99.00 -30.00   82
  5  ω     40.00  65.00   0.50    0.05    --    2.46-138.00  83.00   50
  6  ω     97.00 122.00   0.50    0.06    --   59.04-131.00-101.00   50
  7  ω     39.00 119.00   0.50    0.06    --  115.63-131.00-101.00  160
  8  ω     64.00 123.00   0.50    0.06    --  115.63-138.00  83.00  118
  9  ω    139.00 177.00   0.50    0.06    --  115.63  63.00 120.00   76
 10  ω    101.00 144.00   0.50    0.06    --  115.63 111.00 -60.00   86
 11  ω    110.00 137.00   0.50    0.06    --  115.63 178.00-180.00   54
 12  ω     60.00 104.00   0.50    0.06    --  115.63 178.00-180.00   88
 13  ω     60.00 125.00   0.50    0.06    --  115.63 178.00 -90.00  130
 14  ω     60.00 148.00   0.50    0.06    --  115.63 178.00  30.00  176
 15  ω     72.00 119.00   0.50    0.06    --  115.63  63.00 120.00   94
 16  ω     61.00 113.00   0.50    0.06    --  115.63 178.00  90.00  104
 17  ω    -70.00 -44.00   0.50    0.05    --   -2.46 178.00  30.00   52
 18  ω    -73.00 -48.00   0.50    0.05    --   -2.46 131.00 -29.00   50
 19  ω    -75.00 -50.00   0.50    0.05    --    2.46 138.00 145.00   50
 20  ω   -101.00 -17.00   0.50    0.06    --  -59.04 138.00 145.00  168
 21  ω    -52.00 -27.00   0.50    0.06    -- -106.00 138.00 145.00   50
 22  ω    -87.00 -54.00   0.50    0.06    -- -106.00 111.00 120.00   66
 23  ω   -159.00-104.00   0.50    0.06    -- -106.00 -91.00   0.00  110
 24  ω    -93.00 -68.00   0.50    0.06    --  -59.04-138.00  83.00   50
 25  ω   -137.00 -80.00   0.50    0.06    --  -59.04 -94.00  90.00  114
 26  ω   -162.00 -83.00   0.50    0.06    --  -59.04 -94.00 150.00  158
 27  ω   -162.00-116.00   0.50    0.06    --  -59.04 -94.00 -60.00   92
 28  ω   -110.00 -84.00   0.50    0.06    --  -59.04 -94.00 -60.00   52
 29  ω   -110.00 -84.00   0.50    0.06    --  -59.04 -94.00 -90.00   52
 30  ω   -127.00 -67.00   0.50    0.06    --  -59.04-131.00-101.00  120
 31  ω   -122.00 -89.00   0.50    0.06    --  -59.04 -94.00-180.00   66
 32  ω   -134.00 -72.00   0.50    0.06    -- -106.00-131.00-101.00  124
 33  ω   -106.00 -78.00   0.50    0.06    -- -106.00-111.00-150.00   56
 34  ω   -158.00-133.00   0.50    0.06    --  -59.04 -94.00 -90.00   50
 35  ω   -171.00-144.00   0.50    0.06    -- -106.00-111.00-150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0726480000
_diffrn_orient_matrix_UB_12      0.0597549000
_diffrn_orient_matrix_UB_13      0.0975340000
_diffrn_orient_matrix_UB_21      -0.0390683000
_diffrn_orient_matrix_UB_22      -0.1329480000
_diffrn_orient_matrix_UB_23      0.0407202000
_diffrn_orient_matrix_UB_31      0.1867770000
_diffrn_orient_matrix_UB_32      -0.0046288000
_diffrn_orient_matrix_UB_33      0.0895254000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4226
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.337
_diffrn_reflns_theta_min         4.185
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1848
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1164P)²+1.4680P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1729
_reflns_number_total             1848
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01334b2.cif
_cod_data_source_block           exp_2112
_cod_database_code               7234570
_shelx_shelxl_version_number     2018/3
_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   0.589
_shelx_estimated_absorpt_t_min   0.560
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C3-C5A
 1.48 with sigma of 0.01
3. Restrained planarity
 C5A, O3A, O4A, C3
 with sigma of 0.01
 C3, C5, O3, O4
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O2 \\sim O2A \\sim C1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C5 \\sim O4 \\sim O3 \\sim C5A \\sim O4A \\sim O3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2A) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C5A) \\sim
Ueq, Uanis(O4A) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O2, O2A, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, O4, O3, C5A, O4A, O3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C5A)=Sof(O4A)=Sof(O3A)=0.5*(1-FVAR(2))
 Sof(C5)=Sof(O4)=Sof(O3)=0.5*FVAR(2)
 Sof(O2A)=0.5*(1-FVAR(3))
 Sof(O2)=0.5*FVAR(3)
 Fixed Sof: O10(0.25) O11(0.25) O8(0.25) O9(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.774
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, 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_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 0.36710(9) 0.500000 0.64336(6) 0.0188(3) Uani 1 2 d S T P . .
Cu2 Cu 0.000000 0.36288(7) 0.500000 0.0216(3) Uani 1 2 d S T P . .
O7 O 0.1665(4) 0.500000 0.5045(3) 0.0128(7) Uani 1 2 d S T P . .
O6 O -0.4243(4) 0.3159(3) 0.3928(3) 0.0299(7) Uani 1 1 d . . . . .
O1 O 0.5531(5) 0.500000 0.7921(3) 0.0311(10) Uani 1 2 d S T P A .
O5 O -0.1671(3) 0.2338(3) 0.5053(3) 0.0331(7) Uani 1 1 d . . . . .
C6 C -0.3329(5) 0.2344(3) 0.4583(4) 0.0214(8) Uani 1 1 d . . . . .
C7 C -0.4215(5) 0.1147(4) 0.4822(4) 0.0219(8) Uani 1 1 d . . . . .
C8 C -0.3451(7) 0.000000 0.4664(6) 0.0242(11) Uani 1 2 d S T P . .
H8 H -0.240047 0.000000 0.444687 0.029 Uiso 1 2 calc RS T P . .
C2 C 0.8608(7) 0.500000 0.8932(5) 0.0247(12) Uani 1 2 d S T P A .
O2 O 0.730(2) 0.500000 0.6832(11) 0.027(5) Uani 0.47(5) 2 d S TU P A 2
C1 C 0.7075(7) 0.500000 0.7816(5) 0.0260(12) Uani 1 2 d S TU P . .
C3 C 1.0359(7) 0.500000 0.8884(5) 0.0288(13) Uani 1 2 d DS T P . .
C4 C 1.1726(7) 0.500000 0.9948(5) 0.0308(14) Uani 1 2 d S T P A .
H4 H 1.289277 0.500000 0.991556 0.037 Uiso 1 2 calc RS T P . .
C5 C 1.095(2) 0.525(3) 0.769(2) 0.017(3) Uani 0.27(4) 1 d . U . A -2
O4 O 1.077(4) 0.624(3) 0.725(2) 0.022(4) Uani 0.27(4) 1 d . U . A -2
O3 O 1.158(4) 0.424(3) 0.738(2) 0.024(4) Uani 0.27(4) 1 d . U . A -2
O10 O 0.222(3) 0.224(3) 0.840(2) 0.087(6) Uiso 0.25 1 d . . . . .
O11 O 0.010(4) 0.075(4) 0.709(3) 0.133(11) Uiso 0.25 1 d . . . B 2
O8 O 0.749(4) 0.192(4) 0.790(3) 0.125(10) Uiso 0.25 1 d . . . . .
O9 O 0.970(4) 0.155(3) 0.786(3) 0.113(9) Uiso 0.25 1 d . . . C 1
C5A C 1.091(3) 0.465(4) 0.7806(11) 0.018(4) Uani 0.23(4) 1 d D U . A -1
O4A O 1.194(4) 0.543(3) 0.753(2) 0.019(4) Uani 0.23(4) 1 d . U . A -1
O3A O 1.038(5) 0.358(3) 0.714(3) 0.026(5) Uani 0.23(4) 1 d . U . A -1
O2A O 0.749(2) 0.445(3) 0.6879(12) 0.027(3) Uani 0.26(3) 1 d . U . A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O7 Cu1 O6 90.22(9) . 3_566
O7 Cu1 O6 90.22(9) . 2_556
O7 Cu1 O1 174.50(15) . .
O6 Cu1 O6 140.57(18) 2_556 3_566
O1 Cu1 O6 91.63(9) . 2_556
O1 Cu1 O6 91.63(9) . 3_566
O7 Cu2 Cu2 41.82(7) . 3_566
O7 Cu2 Cu2 41.82(7) 3_566 3_566
O7 Cu2 O7 83.64(14) 3_566 .
O5 Cu2 Cu2 135.64(9) 2_556 3_566
O5 Cu2 Cu2 135.64(9) . 3_566
O5 Cu2 O7 93.91(11) . 3_566
O5 Cu2 O7 175.90(13) . .
O5 Cu2 O7 175.90(14) 2_556 3_566
O5 Cu2 O7 93.91(11) 2_556 .
O5 Cu2 O5 88.72(18) . 2_556
Cu1 O7 Cu2 114.30(11) . .
Cu1 O7 Cu2 114.30(11) . 3_566
Cu2 O7 Cu2 96.36(14) . 3_566
C6 O6 Cu1 131.2(2) . 3_566
C1 O1 Cu1 115.1(3) . .
C6 O5 Cu2 128.3(3) . .
O6 C6 O5 128.2(3) . .
O6 C6 C7 118.7(3) . .
O5 C6 C7 113.0(3) . .
C7 C7 C6 122.92(19) 2_456 .
C8 C7 C6 117.9(3) . .
C8 C7 C7 119.2(2) . 2_456
C7 C8 C7 121.6(5) 4 .
C3 C2 C1 121.8(5) . .
C3 C2 C4 119.1(5) . 3_767
C4 C2 C1 119.1(5) 3_767 .
O1 C1 C2 118.7(4) . .
O1 C1 O2A 122.6(8) . 4_565
O1 C1 O2A 122.6(8) . .
O2 C1 O1 120.0(9) . .
O2 C1 C2 121.3(8) . .
O2 C1 O2A 26.1(11) . 4_565
O2A C1 C2 112.2(9) 4_565 .
O2A C1 C2 112.2(9) . .
O2A C1 O2A 51(2) 4_565 .
C2 C3 C5 124.5(8) . .
C2 C3 C5A 124.2(12) . .
C4 C3 C2 119.2(5) . .
C4 C3 C5 115.4(6) . .
C4 C3 C5A 114.4(9) . .
C3 C4 C2 121.7(5) . 3_767
O4 C5 C3 120(2) . .
O4 C5 O3 130(3) . .
O3 C5 C3 110(2) . .
O4A C5A C3 114(3) . .
O4A C5A O3A 120.7(19) . .
O3A C5A C3 125(3) . .
O2A O2A C1 64.7(11) 4_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O7 1.908(3) .
Cu1 O6 2.066(3) 3_566
Cu1 O6 2.066(3) 2_556
Cu1 O1 1.919(4) .
Cu2 Cu2 2.8968(15) 3_566
Cu2 O7 1.944(2) .
Cu2 O7 1.944(2) 3_566
Cu2 O5 1.907(3) .
Cu2 O5 1.907(3) 2_556
O6 C6 1.234(5) .
O1 C1 1.255(7) .
O5 C6 1.263(5) .
C6 C7 1.508(5) .
C7 C7 1.410(7) 2_456
C7 C8 1.387(4) .
C2 C1 1.498(7) .
C2 C3 1.395(7) .
C2 C4 1.397(7) 3_767
O2 C1 1.205(14) .
C1 O2A 1.350(18) .
C1 O2A 1.350(18) 4_565
C3 C4 1.387(8) .
C3 C5 1.61(2) .
C3 C5A 1.483(10) .
C5 O4 1.16(4) .
C5 O3 1.27(4) .
O11 O11 1.59(7) 4
C5A O4A 1.26(4) .
C5A O3A 1.36(5) .
O2A O2A 1.16(6) 4_565
