Switchable gate-opening effect in metal-organic polyhedra assemblies through solution processing.
Craig, Gavin A.; Larpent, Patrick; Kusaka, Shinpei; Matsuda, Ryotaro; Kitagawa, Susumu; Furukawa, Shuhei; Chemical science 9 (2018) 6463–6469; doi:10.1039/c8sc02263a

data_1549672
_publ_section_title
;
 Switchable gate-opening effect in metal-organic polyhedra assemblies
 through solution processing.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              6463
_journal_page_last               6469
_journal_paper_doi               10.1039/c8sc02263a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C112 H84 Cu4 O24, 10(C4 H8 O)'
_chemical_formula_sum            'C152 H164 Cu4 O34'
_chemical_formula_weight         2788.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.5382(15)
_cell_length_b                   25.3600(16)
_cell_length_c                   19.6509(16)
_cell_measurement_reflns_used    22093
_cell_measurement_temperature    97
_cell_measurement_theta_max      30.0150
_cell_measurement_theta_min      2.3180
_cell_volume                     8297.8(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      97
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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    -67.00 -41.00   0.50   24.00    --    4.00  45.00  30.00   52
  2  \w    -26.00   0.00   0.50   24.00    --    4.00  45.00  90.00   52
  3  \w   -103.00 -37.00   0.50   24.00    --  -13.90  45.00 150.00  132
  4  \w    -52.00  34.00   0.50   24.00    --  -13.90  45.00  60.00  172
  5  \w    -19.00   7.00   0.50   24.00    --  -13.90  45.00 150.00   52
  6  \w   -103.00  75.00   0.50   24.00    --  -13.90  45.00   0.00  356
  7  \w    -73.00 -23.00   0.50   24.00    --  -13.90  45.00 120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0182749000
_diffrn_orient_matrix_UB_12      0.0224061000
_diffrn_orient_matrix_UB_13      -0.0075012000
_diffrn_orient_matrix_UB_21      -0.0200776000
_diffrn_orient_matrix_UB_22      -0.0055411000
_diffrn_orient_matrix_UB_23      -0.0394178000
_diffrn_orient_matrix_UB_31      -0.0328141000
_diffrn_orient_matrix_UB_32      0.0157804000
_diffrn_orient_matrix_UB_33      -0.0031090000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85503
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         17542
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0657P)^2^+6.1153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13755
_reflns_number_total             17542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02263a2.cif
_cod_data_source_block           gac269_sq
_cod_depositor_comments
'Adding full bibliography for 1549671--1549673.cif.'
_cod_database_code               1549672
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 H48 O7 Cu4'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C4A-C3A
 1.52 with sigma of 0.02
 C2A-C3A
 1.52 with sigma of 0.02
 O1A-C2A
 1.48 with sigma of 0.02
 C5A-O1A
 1.48 with sigma of 0.02
 C5T-C4T
 1.48 with sigma of 0.02
 C3C-C2C
 1.52 with sigma of 0.02
 C32E-C4E
 1.52 with sigma of 0.02
 C5E-C4E
 1.52 with sigma of 0.02
 C32E-C22E
 1.52 with sigma of 0.02
 O1E-C5E
 1.42 with sigma of 0.02
 O1E-C22E
 1.42 with sigma of 0.02
 C22E-C32E
 1.48 with sigma of 0.02
 C21E-O1E
 1.42 with sigma of 0.02
 C21E-C31E
 1.48 with sigma of 0.02
 C31E-C4E
 1.52 with sigma of 0.02
 C4E-C32E
 1.52 with sigma of 0.02
 C4E-C5E
 1.5 with sigma of 0.02
 C5E-O1E
 1.48 with sigma of 0.02
3. Rigid bond restraints
 O1E, C5E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22E, O1E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32E, C22E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5E, C4E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32E, C4E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3B, C2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3B, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1E \\sim C5E: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1E \\sim C22E: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C22E \\sim C32E: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C4E \\sim C5E: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C32E \\sim C4E: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C3B \\sim C2B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3B \\sim C4B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(H4EC)=Sof(H4ED)=Sof(C22E)=Sof(H22A)=Sof(H22B)=Sof(C32E)=Sof(H32A)=
 Sof(H32B)=1-FVAR(1)
 Sof(H4EA)=Sof(H4EB)=Sof(C21E)=Sof(H21A)=Sof(H21B)=Sof(C31E)=Sof(H31A)=
 Sof(H31B)=FVAR(1)
6.a Rotating group:
 O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C25(H25A,H25B), C5B(H5BA,H5BB), C2T(H2TA,H2TB), C5T(H5TA,
 H5TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB), C4B(H4BA,H4BB), C5C(H5CA,H5CB),
 C3D(H3DA,H3DB), C2B(H2BA,H2BB), C4D(H4DA,H4DB), C4C(H4CA,H4CB), C3A(H3AA,H3AB),
  C4E(H4EC,H4ED), C4E(H4EA,H4EB), C3B(H3BA,H3BB), C2A(H2AA,H2AB), C2C(H2CA,
 H2CB), C4A(H4AA,H4AB), C2D(H2DA,H2DB), C5A(H5AA,H5AB), C22E(H22A,H22B),
 C3C(H3CA,H3CB), C5D(H5DA,H5DB), C32E(H32A,H32B), C5E(H5EA,H5EB), C21E(H21A,
 H21B), C31E(H31A,H31B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C40(H40), C47(H47), C36(H36), C23(H23), C49(H49), C2(H2), C38(H38),
 C12(H12), C21(H21), C10(H10), C11(H11), C30(H30), C45(H45), C28(H28), C46(H46),
  C37(H37), C32(H32), C4(H4), C6(H6), C20(H20), C19(H19)
6.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              25480
_shelx_fab_checksum              52175
_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 2.491
_oxdiff_exptl_absorpt_empirical_full_min 0.630