Interactions of Small-Molecule Guests with Interior and Exterior Surfaces of a Coordination Cage Host
Taylor, Christopher G. P.; Train, Jennifer S.; Ward, Michael D.; Chemistry 2 (2020) 510–524; doi:10.3390/chemistry2020031

data_1558498
_publ_section_title
;
 Interactions of Small-Molecule Guests with Interior and Exterior Surfaces
 of a Coordination Cage Host
;
_journal_issue                   2
_journal_name_full               Chemistry
_journal_page_first              510
_journal_page_last               524
_journal_paper_doi               10.3390/chemistry2020031
_journal_volume                  2
_journal_year                    2020
_chemical_formula_moiety
'C336 H264 Co8 N72, 6.226(B2 F8), B2 F5, 2.226(C18 H20 O2), 0.415(O2)'
_chemical_formula_sum            'C407.8 H417.66 B16 Co8 F64 N72 O31.03'
_chemical_formula_weight         8684.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-31
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 95.9061(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   32.56923(10)
_cell_length_b                   30.16165(10)
_cell_length_c                   40.83634(17)
_cell_measurement_reflns_used    82761
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.389386785
_cell_measurement_theta_min      0.96825261896
_cell_volume                     39902.3(2)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.12.1-g84e9f68aa-release'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.12.1-g84e9f68aa-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.757-g89e4ddb2-dials-1.12 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            346719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.947
_diffrn_reflns_theta_min         0.987
_diffrn_source                   'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.973202011345
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.065: AIMLESS, version 0.7.3 : 15/08/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             17955
_exptl_crystal_preparation
'Crystal was soaked in a solution of 2[prime]-Methylacetophenone in methanolic mother liquor from the solvothermal crystals growth for 24 hours. Crystals were transferred to Fomblin oil before a crystal was mounted on a MiteGen Microloop and flash frozen under liquid nitrogen for storage.'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.890
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2727
_refine_ls_number_reflns         63534
_refine_ls_number_restraints     7141
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1858P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2704
_refine_ls_wR_factor_ref         0.2981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37629
_reflns_number_total             63534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2MeAcetophenone.cif
_cod_data_source_block           dmwmsv6-25_sq
_cod_depositor_comments
'Adding full bibliography for 1558494--1558498.cif.'
_cod_original_cell_volume        39902.31(19)
_cod_original_formula_sum        'C407.80 H417.66 B16 Co8 F64 N72 O31.03'
_cod_database_code               1558498
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.984
_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
 C23I-O22I \\sim C23H-O22H \\sim C23J-O22J \\sim C23G-O22G
 with sigma of 0.04
 O22I-C21I \\sim O22H-C21H \\sim O22J-C21J \\sim O22G-C21G
 with sigma of 0.02
 C23I-C21I \\sim C23H-C21H \\sim C23J-C21J \\sim C23G-C21G
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31A, C32A, C33A, C34A, C35A, C36A}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41A, N42A, C43A, C44A, C45A}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11B, C12B, C13B, C14B, C15B, C16B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31B, C32B, C33B, C34B, C35B, C36B}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41B, N42B, C43B, C44B, C45B}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C51B, C52B, C53B, C54B, C55B, C56B, C61B, C62B, C63B, C64B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11C, C12C, C13C, C14C, C15C, C16C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21C, N22C, C23C, C24C, C25C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31C, C32C, C33C, C34C, C35C, C36C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41C, N42C, C43C, C44C, C45C}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C51C, C52C, C53C, C54C, C55C, C56C, C61C, C62C, C63C, C64C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11D, C12D, C13D, C14D, C15D, C16D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21D, N22D, C23D, C24D, C25D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31D, C32D, C33D, C34D, C35D, C36D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41D, N42D, C43D, C44D, C45D}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C51D, C52D, C53D, C54D, C55D, C56D, C61D, C62D, C63D, C64D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11E, C12E, C13E, C14E, C15E, C16E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21E, N22E, C23E, C24E, C25E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31E, C32E, C33E, C34E, C35E, C36E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41E, N42E, C43E, C44E, C45E}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C51E, C52E, C53E, C54E, C55E, C56E, C61E, C62E, C63E, C64E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11F, C12F, C13F, C14F, C15F, C16F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21F, N22F, C23F, C24F, C25F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31F, C32F, C33F, C34F, C35F, C36F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41F, N42F, C43F, C44F, C45F}
{C51A, C52A, C53A, C54A, C55A, C56A, C61A, C62A, C63A, C64A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C51F, C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B21, F22, F23, F24, F25}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B21A, F22A, F23A, F24A, F25A}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B31, F32, F33, F34, F35}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B41, F42, F43, F44, F45}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B51, F52, F53, F54, F55}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B51A, F52A, F53A, F54A, F55A}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B61, F62, F63, F64, F65}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B71, F72, F73, F74, F75}
{B11, F12, F14, F13, F15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B71A, F72A, F73A, F74A, F75A}
{B11, F12, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B91, F92, F93}
{C11G, C12G, C13G, C14G, C15G, C16G, C31G, C21G} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11H, C12H, C13H, C14H, C15H, C16H, C31H, C21H}
{C11G, C12G, C13G, C14G, C15G, C16G, C31G, C21G} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11I, C12I, C13I, C14I, C15I, C16I, C31I, C21I}
{C11G, C12G, C13G, C14G, C15G, C16G, C31G, C21G} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11J, C12J, C13J, C14J, C15J, C16J, C31J, C21J}
6. Others
 Sof(C11G)=Sof(C12G)=Sof(C13G)=Sof(H13G)=Sof(C14G)=Sof(H14G)=Sof(C15G)=
 Sof(H15G)=Sof(C16G)=Sof(H16G)=Sof(C31G)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C21G)=Sof(O22G)=Sof(C23G)=Sof(H23G)=Sof(H23H)=Sof(H23I)=FVAR(1)
 Sof(O16)=1-FVAR(2)
 Sof(C11J)=Sof(C12J)=Sof(C13J)=Sof(H13J)=Sof(C14J)=Sof(H14J)=Sof(C15J)=
 Sof(H15J)=Sof(C16J)=Sof(H16J)=Sof(C31J)=Sof(H31J)=Sof(H31K)=Sof(H31L)=
 Sof(C21J)=Sof(O22J)=Sof(C23J)=Sof(H23P)=Sof(H23Q)=Sof(H23R)=FVAR(2)
 Sof(B61)=Sof(F62)=Sof(F63)=Sof(F64)=Sof(F65)=FVAR(3)
 Fixed Sof: B21(0.6) F22(0.6) F23(0.6) F24(0.6) F25(0.6) B21A(0.4) F22A(0.4)
 F23A(0.4) F24A(0.4) F25A(0.4) B51(0.5) F52(0.5) F53(0.5) F54(0.5) F55(0.5)
 B51A(0.5) F52A(0.5) F53A(0.5) F54A(0.5) F55A(0.5) B71(0.5) F72(0.5) F73(0.5)
 F74(0.5) F75(0.5) B71A(0.33333) F72A(0.33333) F73A(0.33333) F74A(0.33333)
 F75A(0.33333) C11H(0.63958) C12H(0.63958) C13H(0.63958) H13H(0.63958)
 C14H(0.63958) H14H(0.63958) C15H(0.63958) H15H(0.63958) C16H(0.63958)
 H16H(0.63958) C31H(0.63958) H31D(0.63958) H31E(0.63958) H31F(0.63958)
 C21H(0.63958) O22H(0.63958) C23H(0.63958) H23J(0.63958) H23K(0.63958)
 H23L(0.63958) C11I(0.36042) C12I(0.36042) C13I(0.36042) H13I(0.36042)
 C14I(0.36042) H14I(0.36042) C15I(0.36042) H15I(0.36042) C16I(0.36042)
 H16I(0.36042) C31I(0.36042) H31G(0.36042) H31H(0.36042) H31I(0.36042)
 C21I(0.36042) O22I(0.36042) C23I(0.36042) H23M(0.36042) H23N(0.36042)
 H23O(0.36042)
7.a Secondary CH2 refined with riding coordinates:
 C26A(H26A,H26B), C46A(H46A,H46B), C26B(H26C,H26D), C46B(H46C,H46D), C26C(H26E,
 H26F), C46C(H46E,H46F), C26D(H26G,H26H), C46D(H46G,H46H), C26E(H26I,H26J),
 C46E(H46I,H46J), C26F(H26K,H26L), C46F(H46K,H46L)
7.b Me refined with riding coordinates:
 C31G(H31A,H31B,H31C), C23G(H23G,H23H,H23I), C31H(H31D,H31E,H31F), C23H(H23J,
 H23K,H23L), C31I(H31G,H31H,H31I), C23I(H23M,H23N,H23O), C31J(H31J,H31K,H31L),
 C23J(H23P,H23Q,H23R)
7.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C23A(H23A), C24A(H24A),
 C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C43A(H43A), C44A(H44A),
 C52A(H52A), C53A(H53A), C54A(H54A), C61A(H61A), C62A(H62A), C63A(H63A),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C23B(H23B), C24B(H24B),
 C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B), C43B(H43B), C44B(H44B),
 C52B(H52B), C53B(H53B), C54B(H54B), C61B(H61B), C62B(H62B), C63B(H63B),
 C13C(H13C), C14C(H14C), C15C(H15C), C16C(H16C), C23C(H23C), C24C(H24C),
 C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C), C43C(H43C), C44C(H44C),
 C52C(H52C), C53C(H53C), C54C(H54C), C61C(H61C), C62C(H62C), C63C(H63C),
 C13D(H13D), C14D(H14D), C15D(H15D), C16D(H16D), C23D(H23D), C24D(H24D),
 C33D(H33D), C34D(H34D), C35D(H35D), C36D(H36D), C43D(H43D), C44D(H44D),
 C52D(H52D), C53D(H53D), C54D(H54D), C61D(H61D), C62D(H62D), C63D(H63D),
 C13E(H13E), C14E(H14E), C15E(H15E), C16E(H16E), C23E(H23E), C24E(H24E),
 C33E(H33E), C34E(H34E), C35E(H35E), C36E(H36E), C43E(H43E), C44E(H44E),
 C52E(H52E), C53E(H53E), C54E(H54E), C61E(H61E), C62E(H62E), C63E(H63E),
 C13F(H13F), C14F(H14F), C15F(H15F), C16F(H16F), C23F(H23F), C24F(H24F),
 C33F(H33F), C34F(H34F), C35F(H35F), C36F(H36F), C43F(H43F), C44F(H44F),
 C52F(H52F), C53F(H53F), C54F(H54F), C61F(H61F), C62F(H62F), C63F(H63F),
 C13G(H13G), C14G(H14G), C15G(H15G), C16G(H16G), C13H(H13H), C14H(H14H),
 C15H(H15H), C16H(H16H), C13I(H13I), C14I(H14I), C15I(H15I), C16I(H16I),
 C13J(H13J), C14J(H14J), C15J(H15J), C16J(H16J)
;
_shelx_res_checksum              40583
_shelx_hkl_checksum              24795
_shelx_fab_checksum              52245
_olex2_submission_original_sample_id v2-25-F42_2MeAcetPh
_olex2_submission_special_instructions 'No special instructions were received'