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_1549673
_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         'C54 H32 O12 Rh2, C54.67 H27 N O12 Rh2'
_chemical_formula_sum            'C108.67 H59 N O24 Rh4'
_chemical_formula_weight         2174.19
_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   geom
_audit_creation_date             2018-03-06
_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                77.3450(10)
_cell_angle_beta                 83.1250(10)
_cell_angle_gamma                61.9470(10)
_cell_formula_units_Z            2
_cell_length_a                   17.9146(2)
_cell_length_b                   18.0902(3)
_cell_length_c                   27.6891(3)
_cell_measurement_reflns_used    77351
_cell_measurement_temperature    92
_cell_measurement_theta_max      30.2100
_cell_measurement_theta_min      1.7810
_cell_volume                     7725.35(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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      92
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_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    8.00    --    4.00  45.00   0.00  356
  2  \w   -113.00  65.00   0.50    8.00    --  -23.60  45.00  -8.94  356
  3  \w   -113.00  65.00   0.50    8.00    --  -23.60  45.00 179.27  356
  4  \w   -113.00  65.00   0.50    8.00    --  -23.60  45.00 120.00  356
  5  \w   -113.00  65.00   0.50    8.00    --  -23.60  45.00 120.00  356
  6  \w    -96.00 -51.00   0.50    8.00    --  -23.60  45.00 120.00   90
  7  \w    -53.00  65.00   0.50    8.00    --  -23.60  45.00  30.00  236
  8  \w     21.00  65.00   0.50    8.00    --  -23.60  45.00  90.00   88
  9  \w    -66.00  60.00   0.50    8.00    --  -23.60  45.00  60.00  252
 10  \w      1.00  64.00   0.50    8.00    --  -23.60  45.00 -18.81  126
 11  \w   -113.00  64.00   0.50    8.00    --  -23.60  45.00 150.00  354
 12  \w   -113.00 -88.00   0.50    8.00    --  -23.60  45.00 173.55   50
 13  \w   -101.00 -75.00   0.50    8.00    --  -23.60  45.00 -18.81   52
;
_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      0.0186593000
_diffrn_orient_matrix_UB_12      0.0223691000
_diffrn_orient_matrix_UB_13      0.0077034000
_diffrn_orient_matrix_UB_21      -0.0103066000
_diffrn_orient_matrix_UB_22      -0.0122733000
_diffrn_orient_matrix_UB_23      0.0249977000
_diffrn_orient_matrix_UB_31      0.0394866000
_diffrn_orient_matrix_UB_32      -0.0373294000
_diffrn_orient_matrix_UB_33      0.0023065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            181555
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.812
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.935
_exptl_crystal_description       plate
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.450
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         31268
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+18.9591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25263
_reflns_number_total             31268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02263a2.cif
_cod_data_source_block           gac281a_sq
_cod_depositor_comments
'Adding full bibliography for 1549671--1549673.cif.'
_cod_original_cell_volume        7725.36(19)
_cod_database_code               1549673
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Rh4 C100 H50 N4 O30'
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 C103-C104
 1.52 with sigma of 0.02
 C13-C12B
 1.38 with sigma of 0.02
 C12A-C13
 1.38 with sigma of 0.02
 C12B-C11B
 1.4 with sigma of 0.02
 C11A-C12A
 1.4 with sigma of 0.02
 C11B-C10B
 1.38 with sigma of 0.02
 C10A-C11A
 1.38 with sigma of 0.02
 C9-C10B
 1.38 with sigma of 0.02
 C9-C10A
 1.38 with sigma of 0.02
 C27B-O20A
 1.36 with sigma of 0.02
 C51B-O20B
 1.42 with sigma of 0.02
 O20A-C51A
 1.42 with sigma of 0.02
 C52B-C51B
 1.52 with sigma of 0.02
 C51A-C52A
 1.52 with sigma of 0.02
 O20B-C27B
 1.36 with sigma of 0.02
 O20A-C27A
 1.36 with sigma of 0.02
 C27A-C28B
 1.38 with sigma of 0.02
 C27A-C32B
 1.38 with sigma of 0.02
 C27B-C32B
 1.38 with sigma of 0.02
 C32B-C27B
 1.38 with sigma of 0.02
 C27B-C28B
 1.38 with sigma of 0.02
 C27A-C28A
 1.38 with sigma of 0.02
 C27A-C32A
 1.38 with sigma of 0.02
 C32B-C31
 1.38 with sigma of 0.02
 C32A-C31
 1.38 with sigma of 0.02
 C28B-C29
 1.38 with sigma of 0.02
 C28A-C29
 1.38 with sigma of 0.02
 C78B-C79
 1.38 with sigma of 0.02
 O13A-C103
 1.42 with sigma of 0.02
 O13B-C103
 1.42 with sigma of 0.02
 C82A-C81
 1.38 with sigma of 0.02
 C82B-C81
 1.38 with sigma of 0.02
 C77A-C82A
 1.38 with sigma of 0.02
 C77B-C82B
 1.38 with sigma of 0.02
 C77A-C78A
 1.38 with sigma of 0.02
 C78B-C77B
 1.38 with sigma of 0.02
 C77A-O13A
 1.36 with sigma of 0.02
 O13B-C77B
 1.36 with sigma of 0.02
 O13B-C104
 2.36 with sigma of 0.04
 O20B-C52B = O13B-C104
 2.35 with sigma of 0.04
3. Rigid bond restraints
 C51A, C52A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51B, C52B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C51A \\sim C52A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C52B \\sim C51B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C12A) = Uanis(C12B)
Uanis(C11B) = Uanis(C11A)
Uanis(C10A) = Uanis(C10B)
Uanis(C28A) = Uanis(C28B)
Uanis(C27A) = Uanis(C27B)
Uanis(C32A) = Uanis(C32B)
Uanis(O20A) = Uanis(O20B)
Uanis(C51A) = Uanis(C51B)
Uanis(C52A) = Uanis(C52B)
5. Others
 Sof(C12B)=Sof(H12B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=FVAR(1)
 Sof(O20B)=Sof(C32B)=Sof(H32B)=Sof(C28B)=Sof(H28B)=Sof(C27B)=Sof(C51B)=
 Sof(H51A)=Sof(H51B)=Sof(C52B)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(2)
 Sof(O20A)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52D)=Sof(H52E)=
 Sof(H52F)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(C32A)=Sof(H32A)=FVAR(2)
 Sof(O13B)=1-FVAR(3)
 Sof(O13A)=FVAR(3)
 Sof(C82B)=Sof(H82B)=Sof(C77B)=Sof(C78B)=Sof(H78B)=1-FVAR(4)
 Sof(C82A)=Sof(H82A)=Sof(C77A)=Sof(C78A)=Sof(H78A)=FVAR(4)
 Fixed Sof: C103(0.33333) C104(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C101(H10C,H10D), C51B(H51A,H51B), C51A(H51C,H51D)
6.b Aromatic/amide H refined with riding coordinates:
 C97(H97), C40(H40), C36(H36), C75(H75), C38(H38), C37(H37), C45(H45),
 C99(H99), C58(H58), C21(H21), C23(H23), C90(H90), C88(H88), C73(H73), C86(H86),
  C95(H95), C66(H66), C14(H14), C96(H96), C71(H71), C56(H56), C6(H6), C30(H30),
 C72(H72), C20(H20), C87(H87), C2(H2), C54(H54), C47(H47), C32B(H32B),
 C28B(H28B), C19(H19), C64(H64), C4(H4), C49(H49), C12B(H12B), C62(H62),
 C48(H48), C63(H63), C80(H80), C82B(H82B), C10B(H10B), C11B(H11B), C10A(H10A),
 C11A(H11A), C12A(H12A), C28A(H28A), C32A(H32A), C78B(H78B), C82A(H82A),
 C78A(H78A)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C102(H10E,H10F,H10G), C52B(H52A,H52B,H52C), C52A(H52D,
 H52E,H52F)
;
_shelx_res_checksum              51874
_shelx_fab_checksum              6644
_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 1.828
_oxdiff_exptl_absorpt_empirical_full_min 0.609