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
Zhang, Jun; Ma, Xiaofan; Kong, Weili; Lu, Guodong; Xuan, Xiaopeng; CrystEngComm  (2019) –; doi:10.1039/C9CE01334B

data_7234570
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00 -19.00   0.50    0.05    --   -2.46  57.00 150.00   62
  2  \w      3.00  29.00   0.50    0.05    --   -2.46  57.00 150.00   52
  3  \w     54.00  80.00   0.50    0.05    --   -2.46  57.00 150.00   52
  4  \w      0.00  41.00   0.50    0.05    --   -2.46 -99.00 -30.00   82
  5  \w     40.00  65.00   0.50    0.05    --    2.46-138.00  83.00   50
  6  \w     97.00 122.00   0.50    0.06    --   59.04-131.00-101.00   50
  7  \w     39.00 119.00   0.50    0.06    --  115.63-131.00-101.00  160
  8  \w     64.00 123.00   0.50    0.06    --  115.63-138.00  83.00  118
  9  \w    139.00 177.00   0.50    0.06    --  115.63  63.00 120.00   76
 10  \w    101.00 144.00   0.50    0.06    --  115.63 111.00 -60.00   86
 11  \w    110.00 137.00   0.50    0.06    --  115.63 178.00-180.00   54
 12  \w     60.00 104.00   0.50    0.06    --  115.63 178.00-180.00   88
 13  \w     60.00 125.00   0.50    0.06    --  115.63 178.00 -90.00  130
 14  \w     60.00 148.00   0.50    0.06    --  115.63 178.00  30.00  176
 15  \w     72.00 119.00   0.50    0.06    --  115.63  63.00 120.00   94
 16  \w     61.00 113.00   0.50    0.06    --  115.63 178.00  90.00  104
 17  \w    -70.00 -44.00   0.50    0.05    --   -2.46 178.00  30.00   52
 18  \w    -73.00 -48.00   0.50    0.05    --   -2.46 131.00 -29.00   50
 19  \w    -75.00 -50.00   0.50    0.05    --    2.46 138.00 145.00   50
 20  \w   -101.00 -17.00   0.50    0.06    --  -59.04 138.00 145.00  168
 21  \w    -52.00 -27.00   0.50    0.06    -- -106.00 138.00 145.00   50
 22  \w    -87.00 -54.00   0.50    0.06    -- -106.00 111.00 120.00   66
 23  \w   -159.00-104.00   0.50    0.06    -- -106.00 -91.00   0.00  110
 24  \w    -93.00 -68.00   0.50    0.06    --  -59.04-138.00  83.00   50
 25  \w   -137.00 -80.00   0.50    0.06    --  -59.04 -94.00  90.00  114
 26  \w   -162.00 -83.00   0.50    0.06    --  -59.04 -94.00 150.00  158
 27  \w   -162.00-116.00   0.50    0.06    --  -59.04 -94.00 -60.00   92
 28  \w   -110.00 -84.00   0.50    0.06    --  -59.04 -94.00 -60.00   52
 29  \w   -110.00 -84.00   0.50    0.06    --  -59.04 -94.00 -90.00   52
 30  \w   -127.00 -67.00   0.50    0.06    --  -59.04-131.00-101.00  120
 31  \w   -122.00 -89.00   0.50    0.06    --  -59.04 -94.00-180.00   66
 32  \w   -134.00 -72.00   0.50    0.06    -- -106.00-131.00-101.00  124
 33  \w   -106.00 -78.00   0.50    0.06    -- -106.00-111.00-150.00   56
 34  \w   -158.00-133.00   0.50    0.06    --  -59.04 -94.00 -90.00   50
 35  \w   -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       '\w 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/[\s^2^(Fo^2^)+(0.1164P)^2^+1.4680P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            c9ce01334b2.cif
_cod_data_source_block           exp_2112
_cod_database_code               7234570
_shelx_shelxl_version_number     2018/3
_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)
;
_shelx_res_checksum              429
_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