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_1549671
_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         'C110 H82 Cu4 N2 O24'
_chemical_formula_sum            'C110 H82 Cu4 N2 O24'
_chemical_formula_weight         2069.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-13
_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                61.811(2)
_cell_angle_beta                 88.110(2)
_cell_angle_gamma                64.125(2)
_cell_formula_units_Z            1
_cell_length_a                   15.9653(3)
_cell_length_b                   17.6910(4)
_cell_length_c                   18.2258(5)
_cell_measurement_reflns_used    32905
_cell_measurement_temperature    93
_cell_measurement_theta_max      29.1160
_cell_measurement_theta_min      2.1070
_cell_volume                     3983.8(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -85.00  93.00   0.50   12.00    --    4.00  45.00 150.00  356
  2  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00  60.00  356
  3  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00  30.00  356
  4  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00 150.00  356
  5  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00 120.00  356
  6  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00 120.00  356
  7  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00 150.00  356
  8  \w   -111.00  67.00   0.50   12.00    --  -22.00  45.00  90.00  356
  9  \w    -13.00  63.00   0.50   12.00    --  -22.00  45.00  90.00  152
 10  \w    -20.00  20.00   0.50   12.00    --  -22.00  45.00  60.00   80
 11  \w    -59.00  67.00   0.50   12.00    --  -22.00  45.00  -8.74  252
;
_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      -0.0503046000
_diffrn_orient_matrix_UB_12      0.0202917000
_diffrn_orient_matrix_UB_13      -0.0058406000
_diffrn_orient_matrix_UB_21      0.0047883000
_diffrn_orient_matrix_UB_22      -0.0476261000
_diffrn_orient_matrix_UB_23      0.0216675000
_diffrn_orient_matrix_UB_31      0.0026064000
_diffrn_orient_matrix_UB_32      -0.0010889000
_diffrn_orient_matrix_UB_33      0.0392893000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            98887
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68038
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.863
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         14398
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0619P)^2^+2.6207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11852
_reflns_number_total             14398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02263a2.cif
_cod_data_source_block           gac269_3_sq
_cod_depositor_comments
'Adding full bibliography for 1549671--1549673.cif.'
_cod_original_cell_volume        3983.81(18)
_cod_database_code               1549671
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Cu4 C100 H48 O25 N4'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.919
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C46-C47
 1.38 with sigma of 0.02
 C47-C48
 1.38 with sigma of 0.02
 C48-C49
 1.38 with sigma of 0.02
 C461-C471
 1.38 with sigma of 0.02
 C471-C481
 1.38 with sigma of 0.02
 C481-C491
 1.38 with sigma of 0.02
 C491-C50
 1.38 with sigma of 0.02
 C44-C45B
 1.16 with sigma of 0.02
 C45B-C46
 1.46 with sigma of 0.02
 C491-C501
 1.38 with sigma of 0.02
 C501-C52
 1.48 with sigma of 0.02
 C49-C50
 1.38 with sigma of 0.02
 C51B-C50
 1.38 with sigma of 0.02
 C50-C52
 1.48 with sigma of 0.02
 C46-C51A
 1.38 with sigma of 0.02
 C51A-C50
 1.38 with sigma of 0.02
 C51B-C501
 1.38 with sigma of 0.02
 C461-C51B
 1.38 with sigma of 0.02
 C45B-C461
 1.45 with sigma of 0.02
 C45A-C46
 1.45 with sigma of 0.02
 C44-C45A
 1.16 with sigma of 0.02
 C45B-C44
 1.16 with sigma of 0.02
 C2D-N1D
 1.45 with sigma of 0.02
 N1D-C3D
 1.48 with sigma of 0.02
3. Rigid bond restraints
 C44, C45B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C44 \\sim C45B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C49) = Uanis(C491)
Uanis(C48) = Uanis(C481)
Uanis(C471) = Uanis(C47)
Uanis(C461) = Uanis(C46)
Uanis(C501) = Uanis(C50)
Uanis(C51B) = Uanis(C51A)
Uanis(C45A) = Uanis(C45B)
5. Others
 Sof(C51B)=Sof(H51B)=Sof(C45B)=Sof(C491)=Sof(H491)=Sof(C461)=Sof(C471)=
 Sof(H471)=Sof(C481)=Sof(H481)=Sof(C501)=1-FVAR(1)
 Sof(C50)=Sof(C46)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(H47)=Sof(C49)=Sof(H49)=
 Sof(C51A)=Sof(H51A)=Sof(C45A)=FVAR(1)
6.a Rotating group:
 O1S(H1SA,H1SB)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C28(H28A,H28B)
6.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C42(H42), C16(H16), C30(H30), C14(H14), C25(H25), C38(H38),
 C40(H40), C4(H4), C12(H12), C23(H23), C51B(H51B), C8(H8), C22(H22), C21(H21),
 C13(H13), C32(H32), C39(H39), C6(H6), C48(H48), C47(H47), C49(H49), C491(H491),
  C471(H471), C481(H481), C51A(H51A), C1D(H1D)
6.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C1(H1A,H1B,H1C), C3D(H3DA,H3DB,H3DC), C2D(H2DA,H2DB,H2DC)
;
_shelx_res_checksum              6658
_shelx_fab_checksum              23442
_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 1.613
_oxdiff_exptl_absorpt_empirical_full_min 0.609