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_1554959
_publ_section_title
;
 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            'C117 H171 B4 N4 O20'
_chemical_formula_weight         1996.81
_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                 90.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   42.193(8)
_cell_length_b                   8.3560(17)
_cell_length_c                   15.630(3)
_cell_measurement_reflns_used    27352
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.411
_cell_measurement_theta_min      2.951
_cell_volume                     5510.1(19)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.835
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27352
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         35.411
_diffrn_reflns_theta_min         2.951
_diffrn_source                   'SPring-8 BL38B1 beamline'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         14644
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1239P)^2^+2.0760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13912
_reflns_number_total             14644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b00747_si_003.cif
_cod_data_source_block           14B01kdn15_03
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1554959
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              25316
_shelx_hkl_checksum              90615