Nestable Tetrakis(spiroborate) Nanocycles.
Danjo, Hiroshi; Hashimoto, Yuhki; Kidena, Yuki; Nogamine, Ayumi; Katagiri, Kosuke; Kawahata, Masatoshi; Miyazawa, Toshifumi; Yamaguchi, Kentaro; Organic letters 17 (2015) 2154–2157; doi:10.1021/acs.orglett.5b00747

data_1554960
_publ_section_title
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 Nestable Tetrakis(spiroborate) Nanocycles.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              2154
_journal_page_last               2157
_journal_paper_doi               10.1021/acs.orglett.5b00747
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C180 H112 B4 D84 N4 O34 S14'
_chemical_formula_weight         3535.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                81.21(3)
_cell_angle_beta                 74.06(3)
_cell_angle_gamma                62.19(3)
_cell_formula_units_Z            1
_cell_length_a                   16.670(3)
_cell_length_b                   17.440(4)
_cell_length_c                   19.659(4)
_cell_measurement_reflns_used    31642
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.544
_cell_measurement_theta_min      1.625
_cell_volume                     4859(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       HKL2000
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Ortep-3 for windows'
_computing_publication_material  Yadokari-XG
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.655
_diffrn_measurement_device_type  'MarMosaic225 (Rayonix)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.870
_diffrn_reflns_Laue_measured_fraction_max 0.655
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31642
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.655
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         32.544
_diffrn_reflns_theta_min         1.625
_diffrn_source                   'SPring-8 BL38B1 beamline'
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.086(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         16254
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.845
_refine_ls_R_factor_all          0.2091
_refine_ls_R_factor_gt           0.1643
_refine_ls_shift/su_max          0.000
_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          0.4341
_refine_ls_wR_factor_ref         0.4745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9444
_reflns_number_total             16254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b00747_si_004.cif
_cod_data_source_block           14B01hsg01_02
_cod_database_code               1554960
_shelxl_version_number           2014-3
_shelx_res_checksum              81529
_shelx_hkl_checksum              16230