Crystal studies of musk compounds. XIII. Molecular structures of 6-formyl-1,1,2,4,4,7-hexamethyltetralin (I) and 6-formyl-1,1,4,4,5,7-hexamethyltetralin (2)
De Ridder, Dirk J. A.; Fraanje, Jan; Goubitz, Kees; Schenk, Henk; Acta Crystallographica Section C 50 (1994) 1962–1966; doi:10.1107/S0108270194002647

data_2010344
_publ_contact_author
;
     Dr. Dirk J.A. De Ridder
     Commission of the European Communities - Joint Research Centre
     European Institute for Transuranium Elements
     Postfach 2340
     D-76125 Karlsruhe
     Germany
;
_publ_section_title
;
 Crystal studies of musk compounds. XIII. Molecular structures of
 6-formyl-1,1,2,4,4,7-hexamethyltetralin (I) and
 6-formyl-1,1,4,4,5,7-hexamethyltetralin (2)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1962
_journal_page_last               1966
_journal_paper_doi               10.1107/S0108270194002647
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C17 H24 O'
_chemical_formula_sum            'C17 H24 O'
_chemical_formula_weight         244.38
_chemical_melting_point          .92E-91
_chemical_name_systematic        6-formyl-1,1,4,4,5,7-hexamethyltetralin
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 95.630(9)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   10.3660(10)
_cell_length_b                   8.7150(10)
_cell_length_c                   15.984(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    252
_cell_measurement_theta_max      43.8
_cell_measurement_theta_min      40.0
_cell_volume                     1437.0(3)
_computing_cell_refinement       'CELCON comparable to Xtal LATCON'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
; Xtal SORTRF (Hall, Spadaccini & Stewart, 1990) and Xtal ADDREF
(Davenport & Hall, 1990)
;
_computing_molecular_graphics    'PEANUT (Hummel, Hauser & B\"urgi, 1990)'
_computing_publication_material
; Xtal BONDLA (Dreissig, Doherty, Stewart & Hall, 1990) and Xtal CIFIO
(Hall, 1990)
;
_computing_structure_refinement  'Xtal CRYLSQ (Olthof-Hazekamp, 1990)'
_computing_structure_solution    'Xtal SIMPEL (Schenk & Hall, 1990)'
_diffrn_ambient_temperature      252.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  'Not available'
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2671
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         64.84
_diffrn_reflns_theta_min         4.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .484
_exptl_absorpt_correction_T_max  1.34
_exptl_absorpt_correction_T_min  .45
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.13
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'block shaped crystal'
_exptl_crystal_F_000             536
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .15
_refine_diff_density_max         .401
_refine_diff_density_min         -.517
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .235
_refine_ls_goodness_of_fit_obs   .235
_refine_ls_hydrogen_treatment
; Only coordinates of H atoms refined, restrained at 1.09 \%A to their
    carrier atom with fixed U~eq~=0.08 \%A^2^. The angles of the H atoms
    attached to C2 and C3 were restrained at 109 \%. H16 (A & B) were not
    refined
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          .099
_refine_ls_R_factor_obs          .099
_refine_ls_shift/esd_max         .389
_refine_ls_shift/esd_mean        .041
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w=1/(7.52 + F~obs~ + 0.0046 F^2^~obs~)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .117
_refine_ls_wR_factor_obs         .117
_reflns_number_observed          2053
_reflns_number_total             2428
_reflns_observed_criterion       refl_observed_if_Inet_>_2.5__sigma(Inet)
_cod_data_source_file            sh1094.cif
_cod_data_source_block           2
_cod_depositor_comments
;
   Site occupancies and disorder asseblies were reconstructed from the
   authors' comments that were (semantically incorrectly) included
   into coordinate list:

   Population parameter of O1A = 0.69 . .
   Population parameter of O1B = 0.31 . .

   The comments are present in the original paper supplementary CIF
   file, sh1094.cif (http://scripts.iucr.org/cgi-bin/sendcif?sh1094sup1)

   Antanas Vaitkus
   2015.02.14

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not available' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/(7.52 + F~obs~ + 0.0046
F^2^~obs~)' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/(7.52 + F~obs~ + 0.0046 F^2^~obs~)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010344