A Copper-Mediated Conjugate Addition Approach to Analogues of Aconitine-Type Diterpenoid Alkaloids.
Doering, Nicolle A.; Kou, Kevin G. M.; Norseeda, Krissada; Lee, Jack C.; Marth, Christopher J.; Gallego, Gary M.; Sarpong, Richmond; The Journal of organic chemistry 83 (2018) 12911–12920; doi:10.1021/acs.joc.8b01967

data_4035397
_publ_section_title
;
 A Copper-Mediated Conjugate Addition Approach to Analogues of
 Aconitine-Type Diterpenoid Alkaloids.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12911
_journal_page_last               12920
_journal_paper_doi               10.1021/acs.joc.8b01967
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C28 H43 N O6 Si'
_chemical_formula_weight         517.72
_chemical_name_common            ND1-064-B2
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_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
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0538(5)
_cell_length_b                   15.9623(5)
_cell_length_c                   11.2628(3)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.29
_cell_measurement_theta_min      2.76
_cell_volume                     2880.03(15)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    ORTEP-32
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_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         2.0
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_diffrn_reflns_limit_l_min       -11
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.357
_diffrn_reflns_theta_min         2.758
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       blade
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_refine_diff_density_max         0.435
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0574P)^2^+3.4105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1362
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_reflns_number_gt                4944
_reflns_number_total             5282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01967_si_002.cif
_cod_data_source_block           beta-10d
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4035397
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              19143
_shelx_hkl_checksum              24722