An exceptionally high boron content supramolecular cuboctahedron
Daniel J. Clingerman; Robert D. Kennedy; Joseph E. Mondloch; Amy A. Sarjeant; Joseph T. Hupp; Omar K. Farha; Chad A. Mirkin; Chem.Commun. 49 (2013) 11485–; doi:10.1039/c3cc44173c

data_7110090
_publ_section_title
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 An exceptionally high boron content supramolecular cuboctahedron
;
_journal_name_full               Chem.Commun.
_journal_page_first              11485
_journal_paper_doi               10.1039/c3cc44173c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C258 H414 B240 Cu24 N6 O120'
_chemical_formula_sum            'C258 H414 B240 Cu24 N6 O120'
_chemical_formula_weight         9639.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2012-12-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   31.498(4)
_cell_length_b                   31.498(4)
_cell_length_c                   81.077(12)
_cell_measurement_temperature    100(2)
_cell_volume                     69662(16)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            103596
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        58.930
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         3.91
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.751564
_exptl_absorpt_correction_T_min  0.636719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0574 before and 0.0464 after correction.
 
For component 2:
 wR2(int) was 0.0661 before and 0.0493 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.689
_exptl_crystal_description       prism
_exptl_crystal_F_000             14580
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         22202
_refine_ls_number_restraints     5193
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1889P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2878
_refine_ls_wR_factor_ref         0.3009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13821
_reflns_number_total             22202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc44173c.txt
_cod_data_source_block           n2332
_cod_database_code               7110090
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H30 of C30, H27 of C27, H25 of C25, H23 of C23, H20 of C20, H17 of C17, H15
  of C15, H13 of C13, H10 of C10, H7 of C7, H5 of C5, H3 of C3, H30A of B30,
  H29 of B29, H22 of B22, H5A of B5, H35A of B35, H6 of B6, H4 of B4, H19 of
  B19, H20C of B20, H25A of B25, H31 of B31, H27A of B27, H10A of B10, H17A of
  B17, H16 of B16, H35 of C35, H41 of C41, H40 of C40, H37 of C37, H33 of C33,
  H9 of B9, H24 of B24, H34 of B34, H33A of B33, H21 of B21, H8 of B8, H14 of
  B14, H38 of B38, H37A of B37, H39 of B39, H36 of B36, H15A of B15, H28 of B28,
   H7A of B7, H23A of B23, H13A of B13, H3A of B3, H11 of B11, H40A of B40, H32
  of B32, H26 of B26, H2 of B2, H18 of B18, H12 of B12, H1 of B1
 At 1.5 times of:
  {H20A,H20B} of O20, {H19A,H19B} of O19, {H18A,H18B} of O18, {H43A,H43B,
  H43C} of C43, {H42A,H42B,H42C} of C42
2. Restrained distances
 C9-B5 - C9-B1 - C9-B2 - C9-B4 - C9-B3 - C10-B5 - C10-B9 - C10-B10 - C10-B6 -
 C10-B1 - C29-B21 - C29-B22 - C29-B23 - C29-B24 - C29-B25 - C30-B26 - C30-B21 -
 C30-B25 - C30-B29 - C30-B30 - C40-B35 - C40-B39 - C40-B40 - C40-B36 - C40-B31
 - C39-B35 - C39-B31 - C39-B32 - C39-B33 - C39-B34 - C19-B11 - C19-B12 - C19-
 B13 - C19-B14 - C19-B15 - C20-B20 - C20-B16 - C20-B11 - C20-B15 - C20-B19
 with sigma of 0.02
 B13-B12 - B17-B12 - B16-B12 - B17-B16 - B20-B16 - B20-B17 - B20-B18 - B18-B17
 - B17-B13 - B18-B13 - B18-B14 - B14-B13 - B19-B14 - B19-B18 - B20-B19 - B19-
 B15 - B15-B14 - B15-B11 - B16-B11 - B12-B11 - B22-B21 - B26-B22 - B26-B21 -
 B27-B26 - B27-B23 - B27-B22 - B23-B22 - B28-B23 - B28-B27 - B30-B27 - B30-B28
 - B30-B29 - B29-B28 - B28-B24 - B29-B24 - B24-B23 - B25-B24 - B29-B25 - B25-
 B21 - B30-B26 - B9-B8 - B9-B10 - B9-B5 - B9-B4 - B5-B4 - B8-B4 - B8-B10 - B8-
 B3 - B4-B3 - B7-B3 - B8-B7 - B7-B2 - B3-B2 - B6-B2 - B2-B1 - B6-B1 - B7-B6 -
 B6-B10 - B7-B10 - B5-B1 - B35-B34 - B34-B33 - B38-B34 - B39-B34 - B39-B38 -
 B38-B33 - B37-B33 - B37-B32 - B37-B36 - B40-B37 - B38-B37 - B40-B38 - B40-B36
 - B36-B32 - B33-B32 - B32-B31 - B36-B31 - B35-B31 - B40-B39
 with sigma of 0.02
3.a Rotating group:
 O18(H18A,H18B), O19(H19A,H19B), O20(H20A,H20B)
3.b Me refined with riding coordinates:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C13(H13), C15(H15), C17(H17), C23(H23), C25(H25),
 C27(H27), C33(H33), C37(H37), C41(H41), C35(H35)
3.d Boron cage BH refined with riding coordinates:
 C10(H10), C20(H20), C30(H30), C40(H40), B16(H16), B17(H17A), B10(H10A),
 B27(H27A), B31(H31), B25(H25A), B20(H20C), B19(H19), B4(H4), B6(H6), B35(H35A),
  B5(H5A), B22(H22), B1(H1), B12(H12), B18(H18), B2(H2), B26(H26), B32(H32),
 B40(H40A), B11(H11), B3(H3A), B13(H13A), B23(H23A), B7(H7A), B28(H28),
 B15(H15A), B36(H36), B39(H39), B37(H37A), B38(H38), B14(H14), B8(H8), B21(H21),
  B33(H33A), B34(H34), B24(H24), B9(H9), B30(H30A), B29(H29)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 43982.1 Ang^3^ [63.1%]
Total electron count / cell = 9643.9
;
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.905
_shelx_hkl_checksum              13070
_shelx_res_checksum              46588
_shelxl_version_number           2012-6