Structure of a mixed crystal of α- and β-pipitzol (1:1), C~15~H~20~O~3~.C~15~H~20~O~3~
Evans, Stephen V.; Yee, Vivien C.; Garcia-Garibay, Miguel; Trotter, James; Acta Crystallographica Section C 50 (1994) 278–281; doi:10.1107/S0108270193009060

data_2009439
_publ_section_title
;
 Structure of a mixed crystal of \a- and \b-pipitzol (1:1),
 C~15~H~20~O~3~.C~15~H~20~O~3~
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              278
_journal_page_last               281
_journal_paper_doi               10.1107/S0108270193009060
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C15 H20 O3, C15 H20 O3'
_chemical_formula_sum            'C30 H40 O6'
_chemical_formula_weight         '248.32 (per molecule)'
_chemical_name_common            '\a- and \b-Pipitzol (1:1)'
_chemical_name_systematic
;
\a-Pipitzol:  [3R-(3\a,3a\b,7\b,8a\a)]-1,2,3,7,8,8a-hexahydro-5-hydroxy-
3,6,8,8-tetramethyl-4H-3a,7-methanoazulene-4,9-dione
and
\b-Pipitzol:  [3R-(3\a,3a\a,7\a,8a\b)]-1,2,3,7,8,8a-hexahydro-5-hydroxy-
3,6,8,8-tetramethyl-4H-3a,7-methanoazulene-4,9-dione
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                99.850(3)
_cell_angle_beta                 109.361(2)
_cell_angle_gamma                98.229(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6729(3)
_cell_length_b                   10.5434(3)
_cell_length_c                   7.3228(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      49
_cell_measurement_theta_min      40
_cell_volume                     677.96(4)
_computing_cell_refinement       CAD-4
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'ORFLS (Busing, Martin & Levy, 1962)'
_computing_structure_solution    'MULTAN80 (Main et al., 1980)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Nonius CAD-4F'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2792
_diffrn_reflns_theta_max         75
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.64
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_meas      1.21
_exptl_crystal_density_method    flotation
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.30
_refine_ls_extinction_coef       3800.0000
_refine_ls_extinction_method     'Becker & Coppens (1974a,b)'
_refine_ls_goodness_of_fit_obs   2.3
_refine_ls_hydrogen_treatment
;refall (except on C10', where H atoms were placed in calculated positions,
since refinement produced unacceptable geometry)
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     '323 (plus 148 H parameters)'
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_obs          0.044
_refine_ls_shift/esd_max         0.1
_refine_ls_shift/esd_mean        0.02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.054
_refine_ls_wR_factor_obs         0.054
_reflns_number_observed          2327
_reflns_number_total             2792
_reflns_observed_criterion       'I > 3\s(I)'
_cod_data_source_file            cd1061.cif
_cod_data_source_block           pipi_1
_cod_depositor_comments
;
 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-01-17

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        677.97(4)
_cod_database_code               2009439