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_1558496
_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, 0.55(C10 H8 N2 S2), 14(B F4), B2 F5, 2.45(C H4 O)'
_chemical_formula_sum
'C380.04 H422.24 B16 Co8 F64 N73.12 O38.44 S1.12'
_chemical_formula_weight         8525.63
_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             2020-03-30
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 96.33120(19)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   32.81236(7)
_cell_length_b                   30.21497(6)
_cell_length_c                   40.09564(8)
_cell_measurement_reflns_used    107538
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.6443017354
_cell_measurement_theta_min      0.977885160056
_cell_volume                     39509.35(14)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.12.5-gf509b3367-release'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.12.5-gf509b3367-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.769-ga0b6e151-dials-1.12 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            348166
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.947
_diffrn_reflns_theta_min         0.991
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.986143370023
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.067: 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    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             17647
_exptl_crystal_preparation
'Crystal was soaked in a solution of 2,2'-Dipyridyldisulfide 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          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2425
_refine_ls_number_reflns         62848
_refine_ls_number_restraints     6404
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1427P)^2^+0.9462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42312
_reflns_number_total             62848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pySSpy.cif
_cod_data_source_block           dmwmsv3-130_f56_pydisulph_sq
_cod_depositor_comments
'Adding full bibliography for 1558494--1558498.cif.'
_cod_original_cell_volume        39509.35(10)
_cod_database_code               1558496
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.960
_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) groups
2. Restrained distances
 O31S-C32S = O41S-C42S
 1.43 with sigma of 0.005
3. Restrained planarity
 C22G, C23G, C24G, C25G, C26G, N21G
 with sigma of 0.05
 C12G, C13G, C14G, C15G, C16G, N11G
 with sigma of 0.05
4. 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
Uanis(C15G) \\sim Ueq, Uanis(C14G) \\sim Ueq, Uanis(C26G) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(S27G) = Uanis(C42S)
5. Rigid body (RIGU) restrains
 N11G, C12G, C13G, C14G, C15G, C16G, S17G, N21G, C22G, C23G, C24G, C25G, C26G,
 S27G
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31A, C32A, C33A, C34A, C35A, C36A}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N41A, N42A, C43A, C44A, C45A}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N11B, C12B, C13B, C14B, C15B, C16B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31B, C32B, C33B, C34B, C35B, C36B}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{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
{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
{N11C, C12C, C13C, C14C, C15C, C16C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N21C, N22C, C23C, C24C, C25C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31C, C32C, C33C, C34C, C35C, C36C}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{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
{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
{N11D, C12D, C13D, C14D, C15D, C16D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N21D, N22D, C23D, C24D, C25D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31D, C32D, C33D, C34D, C35D, C36D}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{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
{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
{N11E, C12E, C13E, C14E, C15E, C16E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N21E, N22E, C23E, C24E, C25E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31E, C32E, C33E, C34E, C35E, C36E}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{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
{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
{N11F, C12F, C13F, C14F, C15F, C16F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N21F, N22F, C23F, C24F, C25F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31F, C32F, C33F, C34F, C35F, C36F}
{N21A, N22A, C23A, C24A, C25A} sigma for 1-2: 0.02, 1-3: 0.04
as
{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
{C51F, C52F, C53F, C54F, C55F, C56F, C61F, C62F, C63F, C64F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N11G, C12G, C13G, C14G, C15G, C16G}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N21G, C22G, C23G, C24G, C25G, C26G}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B21, F22, F23, F24, F25}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B31, F32, F33, F34, F35}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B41, F42, F43, F44, F45}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B51, F52, F53, F54, F55}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B61, F62, F63, F64, F65}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B71, F72, F73, F74, F75}
{B11, F12, F13, F14, F15} sigma for 1-2: 0.02, 1-3: 0.04
as
{B81, F82, F83, F84, F85}
{B11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as
{B91, F92, F93, F94}
7. Others
 Sof(O31S)=Sof(H31S)=Sof(C32S)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(N11G)=Sof(C12G)=Sof(C13G)=Sof(H13G)=Sof(C14G)=Sof(H14G)=Sof(C15G)=
 Sof(H15G)=Sof(C16G)=Sof(H16G)=Sof(S17G)=Sof(N21G)=Sof(C22G)=Sof(C23G)=
 Sof(H23G)=Sof(C24G)=Sof(H24G)=Sof(C25G)=Sof(H25G)=Sof(C26G)=Sof(H26M)=
 Sof(S27G)=FVAR(1)
 Fixed Sof: B61(0.5) F62(0.5) F63(0.5) F64(0.5) F65(0.5) B81(0.5) F82(0.5)
 F83(0.5) F84(0.5) F85(0.5) O41S(0.5) H41S(0.5) C42S(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5)
8.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)
8.b 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), C23G(H23G), C24G(H24G),
 C25G(H25G), C26G(H26M)
8.c Tetrahedral OH refined with riding coordinates:
 O31S(H31S)
8.d Idealised Me refined as rotating group:
 C32S(H32A,H32B,H32C), C42S(H42A,H42B,H42C)
8.e Idealised tetrahedral OH refined as rotating group:
 O41S(H41S)
;
_shelx_res_checksum              8849
_shelx_hkl_checksum              12867
_shelx_fab_checksum              80697
_olex2_submission_special_instructions 'No special instructions were received'