(±)-(4b<i>S</i>,8a<i>R</i>,10a<i>S</i>)-10a-Ethynyl-4b,8,8-trimethyl-3,7-dioxo-3,4b,7,8,8a,9,10,10a-octahydrophenanthrene-2,6-dicarbonitrile
Zheng, Suqing; Resch, Daniel; Honda, Tadashi; Jasinski, Jerry P.; Acta Crystallographica Section E 68 (2012) o3095–o3096; doi:10.1107/S1600536812041244

data_2236563
_publ_section_title
;
 (+-)-(4b<i>S</i>,8a<i>R</i>,10a<i>S</i>)-10a-Ethynyl-4b,8,8-trimethyl-3,7-dioxo-3,4b,7,8,8a,9,10,10a-octahydrophenanthrene-2,6-dicarbonitrile
;
_journal_coeditor_code           QK2041
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3095
_journal_page_last               o3096
_journal_paper_doi               10.1107/S1600536812041244
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C21 H18 N2 O2'
_chemical_formula_moiety         'C21 H18 N2 O2'
_chemical_formula_sum            'C21 H18 N2 O2'
_chemical_formula_weight         330.37
_chemical_name_systematic
;
(+-)-(4b<i>S</i>,8a<i>R</i>,10a<i>S</i>)-10a-Ethynyl-4b,8,8-trimethyl-3,7-
dioxo-3,4b,7,8,8a,9,10,10a-octahydrophenanthrene-2,6-dicarbonitrile
;
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.051(2)
_cell_angle_beta                 96.284(2)
_cell_angle_gamma                92.338(2)
_cell_formula_units_Z            4
_cell_length_a                   7.3012(2)
_cell_length_b                   12.9843(3)
_cell_length_c                   18.4254(4)
_cell_measurement_reflns_used    16712
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      73.1529
_cell_measurement_theta_min      4.0021
_cell_volume                     1727.26(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'WINGX  (Farrugia, 1999)'
_computing_publication_material
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006), PLATON (Spek, 2009)
and
publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Atlas Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33944
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         69.49
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.177
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.4667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                5160
_reflns_number_total             6478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            qk2041.cif
_cod_data_source_block           I
_cod_database_code               2236563
_cod_database_fobs_code          2236563