Synthesis of rac-Lindenene via a thermally induced cyclopropanation reaction.
Fenlon, Thomas W.; Jones, Michael W.; Adlington, Robert M.; Lee, Victor; Organic & biomolecular chemistry 11 (2013) 8026–8029; doi:10.1039/c3ob41716f

data_7153173
_publ_section_title
;
 Synthesis of rac-Lindenene via a thermally induced cyclopropanation
 reaction.
;
_journal_issue                   46
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8026
_journal_page_last               8029
_journal_paper_doi               10.1039/c3ob41716f
_journal_volume                  11
_journal_year                    2013
_chemical_formula_moiety         'C13 H18 O3'
_chemical_formula_sum            'C13 H18 O3'
_chemical_formula_weight         222.28
_chemical_melting_point          ?
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-08-24
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                88.1107(17)
_cell_angle_beta                 79.4709(16)
_cell_angle_gamma                80.956(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8219(2)
_cell_length_b                   9.1724(4)
_cell_length_c                   9.3248(4)
_cell_measurement_reflns_used    2284
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     566.52(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8424
_diffrn_reflns_theta_full        25.238
_diffrn_reflns_theta_max         27.433
_diffrn_reflns_theta_min         5.213
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.001697
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 18.1 23.3 6.85 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1182
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1182
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1880
_reflns_number_total             2444
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.86
_oxford_diffrn_Wilson_scale      0.42
_oxford_refine_ls_r_factor_ref   0.0750
_oxford_refine_ls_scale          1.514(9)
_oxford_reflns_number_all        2444
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title CYPRO
_cod_data_source_file            c3ob41716f.txt
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7153173