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_1554950
_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            'C152.5 H199 B4 N7 O23'
_chemical_formula_weight         2541.42
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.705(2)
_cell_length_b                   28.512(6)
_cell_length_c                   22.406(5)
_cell_measurement_reflns_used    6555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.528
_cell_measurement_theta_min      1.608
_cell_volume                     7387(3)
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_computing_molecular_graphics    'Ortep-3 for Windows'
_computing_publication_material  Yadokari-XG
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_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.742
_diffrn_measurement_device_type  'MX225HE (Rayonix)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
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_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.742
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_number            6555
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_diffrn_reflns_theta_full        24.528
_diffrn_reflns_theta_max         24.528
_diffrn_reflns_theta_min         1.608
_diffrn_source                   'SPring-8 BL38B1 beamline'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             2734
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.258
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_refine_ls_extinction_coef       0.044(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         6416
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      2.617
_refine_ls_R_factor_all          0.1905
_refine_ls_R_factor_gt           0.1828
_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          0.4757
_refine_ls_wR_factor_ref         0.5029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5228
_reflns_number_total             6416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b00747_si_002.cif
_cod_data_source_block           14B02kdn_01
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C152.50 H199 B4 N7 O23'
_cod_database_code               1554950
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              57037
_shelx_hkl_checksum              4341