Diastereoselective Synthesis of Morphan Derivatives by Michael and Hetero-Michael Addition of 1,1-Enediamines to Quinone Monoketals.
Hu, Xing-Mei; Luo, Da-Yun; Zi, Quan-Xing; Lin, Jun; Yan, Sheng-Jiao; ACS omega 3 (2018) 8–21; doi:10.1021/acsomega.7b01493

data_4515907
_publ_section_title
;
 Diastereoselective Synthesis of Morphan Derivatives by Michael and
 Hetero-Michael Addition of 1,1-Enediamines to Quinone Monoketals.
;
_journal_issue                   1
_journal_name_full               'ACS omega'
_journal_page_first              8
_journal_page_last               21
_journal_paper_doi               10.1021/acsomega.7b01493
_journal_volume                  3
_journal_year                    2018
_chemical_formula_sum            'C17 H21 N3 O5'
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_atom_sites_solution_hydrogens   geom
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_cell_angle_gamma                90
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_cell_length_c                   12.926(19)
_cell_measurement_reflns_used    1057
_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      2.3612
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_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0959
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_diffrn_reflns_Laue_measured_fraction_max 0.999
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_diffrn_reflns_limit_k_max       9
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_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_min         2.361
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_exptl_absorpt_correction_T_min  0.982
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_exptl_absorpt_process_details   sadabs
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_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.200
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_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                1603
_reflns_number_total             3222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b01493_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515907
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2014-3
_shelx_res_checksum              92727
_shelx_hkl_checksum              96623