Carborane inclusion chemistry for the uncommon calix[7,9]arenes
Clark, Thomas E.; Makha, Mohamed; Sobolev, Alexandre N.; Raston, Colin L.; Dalton Transactions  (2008) 4855–4859; doi:10.1039/b807511e

data_7004463
_publ_section_title
;
 Carborane inclusion chemistry for the uncommon calix[7,9]arenes
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4855
_journal_page_last               4859
_journal_paper_doi               10.1039/b807511e
_journal_year                    2008
_chemical_formula_moiety
'2(C99 H126 O9), 7(C2 H12 B10), 2(C6 H12), 5(H2 O)'
_chemical_formula_sum            'C224 H370 B70 O23'
_chemical_formula_weight         4187.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 95.833(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            1
_cell_length_a                   12.2461(9)
_cell_length_b                   30.9771(9)
_cell_length_c                   19.4645(8)
_cell_measurement_reflns_used    4892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.99
_cell_measurement_theta_min      2.69
_cell_volume                     7345.6(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47574
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         12710
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.2129
_refine_ls_R_factor_gt           0.1337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3489
_refine_ls_wR_factor_ref         0.3837
_reflns_number_gt                5071
_reflns_number_total             12710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807511e.txt
_cod_data_source_block           Complex1
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7004463