Rotation barriers in aryl- and heteroaryldi(1-adamantyl)methyl systems; the ionic hydrogenation of heteroaryldi(1-adamantyl)methanols
Lomas, John S.; Lacroix, Jean-Christophe; Vaissermann, Jacqueline; Journal of the Chemical Society, Perkin Transactions 2  (1999) 2001–; doi:10.1039/a905455c

data_7213150
_publ_contact_author
;
  John S. Lomas                       
;
_publ_section_title
;
 Rotation barriers in aryl- and heteroaryldi(1-adamantyl)methyl systems;
 the ionic hydrogenation of heteroaryldi(1-adamantyl)methanols
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2001
_journal_paper_doi               10.1039/a905455c
_journal_year                    1999
_chemical_compound_source
;
direct synthesis by lithiation of 3-methylfuran followed by reaction with
 diadamantyl ketone and separation from the 4-methylfuranyl derivative by
 chromatography and crystallization
;
_chemical_formula_moiety         ' C26 H36 O2 '
_chemical_formula_sum            'C26 H36 O2'
_chemical_formula_weight         380.57
_chemical_melting_point          442.15
_chemical_name_systematic
;
anti[2-(3-methylfuranyl)]di(1-adamantyl)methanol
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   ' located on a difference Fourier map '
_atom_sites_solution_primary     direct
_audit_creation_date             98-10-01
_audit_creation_method           CRYSTALS
_cell_angle_alpha                68.89(4)
_cell_angle_beta                 87.16(5)
_cell_angle_gamma                80.26(3)
_cell_formula_units_Z            2
_cell_length_a                   6.663(4)
_cell_length_b                   11.047(3)
_cell_length_c                   15.062(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      12.9
_cell_volume                     1019.3(9)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      295
_diffrn_measurement_device       '  Enraf-Nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  ' graphite '
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3899
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        12.2
_diffrn_standards_interval_time  3600s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.07
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             416.09
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.29
_refine_ls_extinction_coef       31.57
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.1759
_refine_ls_hydrogen_treatment
;
 one overall isotropic thermal parameter refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2289
_refine_ls_R_factor_obs          0.0734
_refine_ls_shift/esd_max         0.003814
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0846
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              13
_reflns_limit_k_min              -11
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_observed          2289
_reflns_number_total             3563
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            905455csup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '295K' was changed to '295' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '295K' was changed
to '295' - the value should be numeric and without a unit
designator.

'_chemical_melting_point' value '169C' was changed to
'442.15' - it was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Triclinic ' changed to
'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value ' none' changed
to 'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_matrix_type' value ' full ' changed to
'full' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value ' Direct_Methods ' was changed
to 'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1019.2(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C26 H36 O2 '
_cod_database_code               7213150