Unusual thermolysis of aza-cyclic allene under microwave conditions: crystal structure of (3<i>RS</i>,3a<i>SR</i>,8<i>RS</i>,8a<i>RS</i>)-methyl 5,6-dimeth-oxy-3a,10-dimethyl-1-phenyl-3,3a,8,8a-tetra-hydro-3,8-(epimino-methano)-cyclo-penta-[<i>a</i>]indene-2-carboxyl-ate from synchrotron X-ray diffraction.
Anh, Le Tuan; Titov, Alexander A.; Kobzev, Maxim S.; Voskressensky, Leonid G.; Varlamov, Alexey V.; Dorovatovskii, Pavel V.; Khrustalev, Victor N.; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1770–1773; doi:10.1107/S2056989017014864

data_2311488
_publ_section_title
;
 Unusual thermolysis of aza-cyclic allene under microwave conditions:
 crystal structure of
 (3<i>RS</i>,3a<i>SR</i>,8<i>RS</i>,8a<i>RS</i>)-methyl
 5,6-dimeth-oxy-3a,10-dimethyl-1-phenyl-3,3a,8,8a-tetra-hydro-3,8-(epimino-methano)-cyclo-penta-[<i>a</i>]indene-2-carboxyl-ate
 from synchrotron X-ray diffraction.
;
_journal_coeditor_code           YK2110
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1770
_journal_page_last               1773
_journal_paper_doi               10.1107/S2056989017014864
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C25 H27 N O4'
_chemical_formula_sum            'C25 H27 N O4'
_chemical_formula_weight         405.47
_chemical_name_systematic
;(3<i>RS</i>,3a<i>SR</i>,8<i>RS</i>,8a<i>RS</i>)-Methyl
5,6-dimethoxy-3a,10-dimethyl-1-phenyl-3,3a,8,8a-tetrahydro-3,8-(epiminomethano)cyclopenta[<i>a</i>]indene-2-carboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 95.09(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   26.404(5)
_cell_length_b                   7.9303(16)
_cell_length_c                   30.720(6)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.6
_cell_volume                     6407(2)
_computing_cell_refinement
;
<i>i</i>MOSFLM (Battye <i>et al.</i>,  2011)
;
_computing_data_collection
;
<i>Marccd</i> (Doyle, 2011)
;
_computing_data_reduction
;
<i>i</i>MOSFLM (Battye <i>et al.</i>,  2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            74044
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         39.706
_diffrn_reflns_theta_min         3.513
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>Scala</i>; Evans, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.378
_refine_ls_extinction_coef       0.00120(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         13622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.8571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                10086
_reflns_number_total             13622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2110sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2311488
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              14402
_shelx_res_checksum              23040
_shelxl_version_number           2014/6