(+)-syn-Benzotriborneol an enantiopure C(3)-symmetric receptor for water.
Fabris, Fabrizio; De Lucchi, Ottorino; Nardini, Ilaria; Crisma, Marco; Mazzanti, Andrea; Mason, Sax A.; Lemée-Cailleau, Marie-Hélène; Scaramuzzo, Francesca A.; Zonta, Cristiano; Organic & biomolecular chemistry 10 (2012) 2464–2469; doi:10.1039/c2ob06774a

data_7152250
_publ_section_title
;
 (+)-syn-Benzotriborneol an enantiopure C(3)-symmetric receptor for water.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2464
_journal_page_last               2469
_journal_paper_doi               10.1039/c2ob06774a
_journal_volume                  10
_journal_year                    2012
_chemical_formula_sum            'C30 H47 O5.5'
_chemical_formula_weight         495.70
_chemical_name_common
;
(1R,2R,4S,5R,6R,8S,9R,10R,12S)-3,4,7,8,11,12-hexahydro-2,6,10-
trihydroxy-1,5,9,13,13',14,14',15,15'-nonamethyl-1,4:5,8:9,12-
trimethanotriphenylene x 2.5 H2O
;
_chemical_name_systematic
;
(1R,2R,4S,5R,6R,8S,9R,10R,12S)-3,4,7,8,11,12-hexahydro-2,6,10-trihydroxy-
1,5,9,13,13',14,14',15,15'-nonamethyl-1,4:5,8:9,12-trimethanotriphenylene
x 2.5 H2O
;
_space_group_IT_number           179
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   10.8602(10)
_cell_length_b                   10.8602(10)
_cell_length_c                   81.052(10)
_cell_measurement_reflns_used    2587
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      61.71
_cell_measurement_theta_min      3.10
_cell_volume                     8278.9(15)
_computing_cell_refinement       'ILL Rafd19 '
_computing_data_collection       'ILL Mad'
_computing_data_reduction        'ILL Retreat '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      20(2)
_diffrn_detector_area_resol_mean '1.56mm vert, 2.50mm horiz'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'ILL D19 position-sensitive detector 4-circle diffractometer'
_diffrn_measurement_method       'omega step-scans '
_diffrn_radiation_monochromator  Cu220
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux reactor, H1 thermal beam'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.45970
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       97
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            14723
_diffrn_reflns_theta_full        61.86
_diffrn_reflns_theta_max         61.86
_diffrn_reflns_theta_min         4.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '3 hours'
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   'gaussian, and attenuation by Displex cans'
_exptl_absorpt_process_details   'programs D19abs, D19abscan '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated hexagonal pyramid'
_exptl_crystal_F_000             '667 fermi'
_exptl_crystal_size_max          4.0
_exptl_crystal_size_mid          4.0
_exptl_crystal_size_min          2.7
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_coef       0.00074(8)
_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   1.142
_refine_ls_hydrogen_treatment    'full anisotropic refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         4878
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          1.207
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+112.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                4512
_reflns_number_total             4878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob06774a.txt
_cod_data_source_block           mc41n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8278.8(15)
_cod_original_formula_sum        'C30 H47 O5.50'
_cod_database_code               7152250