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_7046891
_publ_section_title
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 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
'C42 H69 N6 Ni4 O13, C42 H68 N6 Ni4 O13, Cl O4, 5(C H4 O), Cl0.5 O1.75, 0.5(Cl)'
_chemical_formula_sum            'C89 H157 Cl2 N12 Ni8 O36.75'
_chemical_formula_weight         2523.84
_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             2018-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
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2018-06-20 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.79(3)
_cell_angle_beta                 92.92(3)
_cell_angle_gamma                90.57(3)
_cell_formula_units_Z            2
_cell_length_a                   15.900(3)
_cell_length_b                   17.230(3)
_cell_length_c                   21.830(4)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      0.935
_cell_volume                     5969.4(19)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            107927
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.935
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             2654
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.199
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         20649
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0720P)^2^+77.2296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18642
_reflns_number_total             20649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01911h2.cif
_cod_data_source_block           K1_sq
_cod_depositor_comments
'Adding full bibliography for 7046891--7046893.cif.'
_cod_original_cell_volume        5969(2)
_cod_database_code               7046891
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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, All O(H) groups
2. Restrained distances
 C69A-C68 \\sim C69B-C68
 with sigma of 0.02
 C70A-C69A \\sim C70B-C69B
 with sigma of 0.02
 C71A-C70A \\sim C71B-C70B
 with sigma of 0.02
 N11-C71B \\sim N11-C71A
 with sigma of 0.02
 Cl2-O14S \\sim Cl2-O15S \\sim Cl2-O13S \\sim Cl2-O16S
 with sigma of 0.02
 Cl1-O10S \\sim Cl1-O9S \\sim Cl1-O12S \\sim Cl1-O11S
 with sigma of 0.02
3. Rigid bond restraints
 O13S, O14S, O15S, O16S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9S, O10S, O11S, O12S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O13S \\sim O14S \\sim O15S \\sim O16S: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O9S \\sim O10S \\sim O11S \\sim O12S: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C69A) = Uanis(C69B) = Uanis(C70B) = Uanis(C70A) = Uanis(C71A) =
Uanis(C71B)
5. Others
 Fixed Sof: H11(0.5) H11A(0.5) H68A(0.5) H68B(0.5) C69A(0.5) H69A(0.5)
 H69B(0.5) C70A(0.5) H70A(0.5) H70B(0.5) C71A(0.5) H71A(0.5) H71B(0.5)
 C69B(0.5) H69C(0.5) H69D(0.5) C70B(0.5) H70C(0.5) H70D(0.5) C71B(0.5)
 H71C(0.5) H71D(0.5) O9S(0.5) O10S(0.5) O11S(0.5) O12S(0.5) O13S(0.5) O14S(0.5)
 O15S(0.5) O16S(0.5) Cl3(0.5) O1A(0.25) O1C(0.5) O2C(0.5) O3C(0.5) Cl4(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6A,H6B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B),
 C4(H4C,H4D), C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), N8(H8A,H8B), N10(H10A,H10B), N12(H12A,H12B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C67(H67A,H67B), C68(H68A,H68B), C69A(H69A,H69B), C70A(H70A,H70B),
 C71A(H71A,H71B), C69B(H69C,H69D), C70B(H70C,H70D), C71B(H71C,H71D)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N5(H5), C8(H8), C9(H9A), C10(H10), C11(H11B), C20(H20),
 C21(H21), C22(H22), C23(H23), C32(H32), C33(H33), C34(H34), C35(H35), N7(H7),
 N9(H9), N11(H11), N11(H11A), C50(H50), C51(H51), C52(H52), C53(H53), C62(H62),
 C63(H63), C64(H64), C65(H65), C74(H74), C75(H75), C76(H76), C77(H77)
6.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,
 H4SC), C7S(H7SA,H7SB,H7SC), C8S(H8SA,H8SB,H8SC)
6.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S), O4S(H4S), O7S(H7S), O8S(H8S)
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_shelx_res_checksum              61495
_shelx_fab_checksum              66300
_olex2_submission_special_instructions 'No special instructions were received'