Ethyl (1<i>R</i>,4<i>S</i>,5<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>)-5,9,13-trimethyl-14-methylene-14-oxotetracyclo[11.2.1.0^1,10^.0^4,9^]hexadecane-5-carboxylate
Shi, Hao; Acta Crystallographica Section E 66 (2010) o154–; doi:10.1107/S1600536809053380

data_2224612
_publ_section_title
;Ethyl
 (1<i>R</i>,4<i>S</i>,5<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>)-5,9,13-trimethyl-14-methylene-14-oxotetracyclo[11.2.1.0^1,10^.0^4,9^]hexadecane-5-carboxylate
;
_journal_coeditor_code           DN2514
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o154
_journal_paper_doi               10.1107/S1600536809053380
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H34 O3'
_chemical_formula_moiety         'C22 H34 O3'
_chemical_formula_sum            'C22 H34 O3'
_chemical_formula_weight         346.49
_chemical_name_systematic
;
Ethyl (1<i>R</i>,4<i>S</i>,5<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>)-5,9,13-
trimethyl-14-methylene-14-oxotetracyclo[11.2.1.0^1,10^.0^4,9^]hexadecane-
5-carboxylate
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.1740(10)
_cell_angle_beta                 87.518(2)
_cell_angle_gamma                79.0180(10)
_cell_formula_units_Z            2
_cell_length_a                   6.5365(9)
_cell_length_b                   12.5639(15)
_cell_length_c                   13.1212(16)
_cell_measurement_reflns_used    1056
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.346
_cell_measurement_theta_min      3.164
_cell_volume                     988.4(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and <i>PLATON</i>
(Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5226
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         3451
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1087P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1889
_reflns_number_gt                1824
_reflns_number_total             3451
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2514.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2224612
_cod_database_fobs_code          2224612