Creating capsules with cubanes.
Kusumoto, Sotaro; Kobayashi, Fumiya; Ohtani, Ryo; Zhang, Yingjie; Harrowfield, Jack; Kim, Yang; Hayami, Shinya; Nakamura, Masaaki; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9575–9578; doi:10.1039/c8dt01911h

data_7046893
_publ_section_title
;
 Creating capsules with cubanes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9575
_journal_page_last               9578
_journal_paper_doi               10.1039/c8dt01911h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C78 H132 N12 Ni8 O26, B F4'
_chemical_formula_sum            'C78 H132 B F4 N12 Ni8 O26'
_chemical_formula_weight         2210.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   21.433(4)
_cell_length_b                   22.146(4)
_cell_length_c                   35.041(7)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      0.979
_cell_volume                     16146(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1645
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            197202
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.979
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             6941
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.244
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1745
_refine_ls_number_reflns         28347
_refine_ls_number_restraints     2224
_refine_ls_restrained_S_all      3.203
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_gt           0.1004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1791P)^2^+38.8623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2613
_refine_ls_wR_factor_ref         0.3296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13887
_reflns_number_total             28347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01911h2.cif
_cod_data_source_block           p21byc_a_sq
_cod_depositor_comments
'Adding full bibliography for 7046891--7046893.cif.'
_cod_database_code               7046893
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of O26, {H24A,H24B} of O24, {H20A,H20B} of O20,
   {H19A,H19B} of O19, {H38A,H38B} of O38, All C(H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H25A,H25B} of O25, {H18A,H18B} of O18, {H37C,H37D} of
  O37, {H39A,H39B} of O39
2. Restrained distances
 C47-C48
 1.542 with sigma of 0.02
 H25B-O23
 2 with sigma of 0.02
 H18A-O11
 2 with sigma of 0.02
 H37C-O32
 2 with sigma of 0.02
 H39A-O34
 2 with sigma of 0.02
 H3-H19
 2 with sigma of 0.02
 H19-H90
 2 with sigma of 0.02
 F4-B1 \\sim F3-B1 \\sim F1-B1 \\sim F2-B1
 with sigma of 0.02
3. Rigid bond restraints
 F2, F3, F4, F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F2 \\sim F3 \\sim F4 \\sim F1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(N14) = Uanis(N16) = Uanis(N18)
Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84)
5. 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
6. Others
 Fixed Sof: F2(0.5) F3(0.5) F4(0.5) F1(0.5)
7.a Riding coordinates:
 O19(H19A,H19B), O20(H20A,H20B), O24(H24A,H24B), O26(H26A,H26B), N1(H1),
 N2(H2A,H2B), N3(H3), N4(H4A,H4B), N5(H5A,H5B), N6(H6), N7(H7), N8(H8A,H8B),
 N9(H9A,H9B), N10(H10), N11(H11), N12(H12A,H12B), O38(H38A,H38B), N13(H13),
 N14(H14A,H14B), N15(H15), N16(H16A,H16B), N17(H17A), N18(H18C,H18D)
7.b Rotating group:
 O18(H18A,H18B), O25(H25A,H25B), O37(H37C,H37D), O39(H39A,H39B)
7.c Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3A,H3B), C4(H4C,H4D), C5(H5C,H5D), C6(H6A,H6B), C9(H9C,H9D),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12C,H12D), C13(H13A,H13B), C20(H20C,H20D),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24C,H24D), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,
 H63B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),
  C97(H97A,H97B), C106(H10F,H10G), C107(H10H,H10I), C108(H10J,H10K), C109(H10L,
 H10M), C110(H11C,H11D)
7.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C28(H28), C29(H29), C30(H30),
 C31(H31), C40(H40), C41(H41), C42(H42), C43(H43), C52(H52), C53(H53), C54(H54),
  C55(H55), C66(H66), C67(H67), C68(H68), C69(H69), C72(H72), C73(H73),
 C74(H74), C75(H75), C87(H87), C88(H88), C89(H89), C90(H90), C100(H100),
 C101(H101), C102(H102), C103(H103), C113(H113), C114(H114), C115(H115),
 C116(H116)
7.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C91(H91A,H91B,H91C),
 C104(H10C,H10D,H10E), C117(H11E,H11F,H11G)
;
_shelx_res_checksum              8537
_shelx_fab_checksum              70626
_olex2_submission_special_instructions 'No special instructions were received'