Dynamic selection in metallo-organic cube Cd<sup>II</sup> <sub>8</sub>L<sub>4</sub> conformations induced by perfluorooctanoate encapsulation.
Li, Yu-Qing; Zhao, He; Han, Ermeng; Jiang, Zhiyuan; Bai, Qixia; Guan, Yu-Ming; Zhang, Zhe; Wu, Tun; Wang, Pingshan; Chemical science 16 (2024) 364–370; doi:10.1039/d4sc07105k

data_1573256
_publ_section_title
;
 Dynamic selection in metallo-organic cube Cd<sup>II</sup>
 <sub>8</sub>L<sub>4</sub> conformations induced by perfluorooctanoate
 encapsulation.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              364
_journal_page_last               370
_journal_paper_doi               10.1039/d4sc07105k
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         '2(C380 H282 Cd8 N48 O8)'
_chemical_formula_sum            'C760 H564 Cd16 N96 O16'
_chemical_formula_weight         13095.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-09-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.333(3)
_cell_length_b                   43.635(4)
_cell_length_c                   40.669(4)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    101.00
_cell_measurement_theta_max      31.916
_cell_measurement_theta_min      2.488
_cell_volume                     50280(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            128000
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        34.144
_diffrn_reflns_theta_max         34.144
_diffrn_reflns_theta_min         1.873
_diffrn_source_current           2.86
_diffrn_source_power             0.20005699999999998
_diffrn_source_voltage           69.95
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.35
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.865
_exptl_crystal_description       block
_exptl_crystal_F_000             13384
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     930
_refine_ls_restrained_S_all      1.732
_refine_ls_R_factor_all          0.1581
_refine_ls_R_factor_gt           0.1346
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3925
_refine_ls_wR_factor_ref         0.4217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5350
_reflns_number_total             7640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07105k2.cif
_cod_data_source_block           t
_cod_depositor_comments          'Adding full bibliography for 1573256.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1573256
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.652
_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
 C03V-C05P
 1.54 with sigma of 0.001
 C04X-C07E
 1.54 with sigma of 0.001
 C03N-C01I
 1.54 with sigma of 0.001
 C00V-C016
 1.54 with sigma of 0.001
 C03J-C04G
 1.54 with sigma of 0.001
 H06P-H07C
 1.9 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O063 \\sim C074 \\sim C062 \\sim C06V \\sim C04D \\sim C071 \\sim C05Z \\sim
C06P: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
C48 \\sim N04S \\sim C07G \\sim C21 \\sim C1 \\sim C084: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
C068 \\sim C05S \\sim C01Y \\sim C033 \\sim N00X \\sim C01W: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
N00L \\sim C03J \\sim C03R \\sim C02U \\sim C00N \\sim C01M: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
4. Rigid body (RIGU) restrains
 C074, O063, C062, C06P, C05Z, C04D, C06V, C071, C056, C04B, C04E, N1, C04X,
 C04R
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C034, C04L, C05E, C04G, N00U, C039, C046, C052, C06B, C06K, C06F, N01Q, C03J,
 C03R, C02U, C00N, C01M, N00L
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01B, C01N, C016, C00W, C00V, C00Y, C02C, C010, C00M, C01D, C01Z, C03X, C061,
 N00S, C02K, C03N, C013, N04S, C48, C084, C1, C21, C07G, C01I, N00Q, C02D, C03H,
  C01V, C041, C055
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C02R, C013, C01F, C050, C01Y, C033, N00X, C01W, C05S, C068, C01K, C01R, C02P,
 C02B, C02G, C02S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C02J, C02F, C026, C04P, C03V
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C56, C07I, C05P, C07W, C05H, C04N
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01T, C029, C04Z, C04W, C03D, C030
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N05A, C06J, C058, C05M, C06U, C07E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Cd01, N6, N00I, N00C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C03I, C04K, C049, C02Y, C02E, C03O, O009, C04T
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H02A(0.5) H02B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C04W(H04A,H04C), C56(H56A,H56B), C02R(H02A,H02B)
6.b Aromatic/amide H refined with riding coordinates:
 C04R(H04R), C04B(H04B), C01M(H01M), C02U(H02U), C03R(H03R), C06J(H06J),
 C058(H058), C05M(H05M), C06U(H06U), C01T(H01T), C03D(H03D), C04P(H04P),
 C02F(H02F), C00M(H00M), C02K(H02K), C03X(H03X), C00W(H00W), C00Y(H00Y),
 C01D(H01D), C034(H034), C05E(H05E), C084(H084), C1(H1), C21(H21), C07G(H07G),
 C01V(H01V), C03H(H03H), C02D(H02D), C01N(H01N), C06F(H06F), C06K(H06K),
 C06B(H06B), C052(H052), C01R(H01R), C068(H068), C05S(H05S), C033(H033),
 C02C(H02C), C03O(H03O), C02Y(H02Y), C049(H049), C03I(H03I), C02G(H02G),
 C02P(H02P), C02S(H02S), C06V(H06V), C071(H071), C06P(H06P), C05Z(H05Z),
 C04N(H04N), C05H(H05H), C050(H050)
6.c Fitted hexagon refined as free rotating group:
 N1(C04X,C04R,C056,C04B,C04E), N00L(C01M,C00N,C02U,C03R,C03J), N05A(C06J,C058,
 C05M,C06U,C07E), C48(C084,C1,C21,C07G,N04S), C046(N01Q,C06F,C06K,C06B,C052),
 C01W(C068,C05S,C01Y,C033,N00X), C03O(C02E,C02Y,C049,C04K,C03I), C04D(C06V,C071,
 C062,C06P,C05Z)
6.d Idealised Me refined as rotating group:
 C04T(H04D,H04E,H04F), C04Z(H04G,H04H,H04I), C055(H05A,H05B,H05C), C074(H07A,
 H07B,H07C), C07W(H07D,H07E,H07F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33999
_shelx_fab_checksum              88164
_olex2_submission_special_instructions 'No special instructions were received'