Base-controlled [3+3] cycloaddition of isoquinoline N-oxides with azaoxyallyl cations.
An, Yuanyuan; Xia, Hongguang; Wu, Jie; Chemical communications (Cambridge, England) 52 (2016) 10415–10418; doi:10.1039/c6cc03650c

data_7124681
_publ_section_title
;
 Base-controlled [3+3] cycloaddition of isoquinoline N-oxides with
 azaoxyallyl cations.
;
_journal_issue                   68
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10415
_journal_page_last               10418
_journal_paper_doi               10.1039/c6cc03650c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C26 H24 N2 O3'
_chemical_formula_weight         412.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-30 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.510(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   12.158(4)
_cell_length_c                   9.715(3)
_cell_measurement_reflns_used    2695
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.70
_cell_volume                     4506(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15292
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.768
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
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_exptl_crystal_description       stick
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0957P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1817
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           mo_51229a
_cod_original_sg_symbol_H-M      'C 2/c'
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_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-2
_shelx_res_checksum              8073