Modular Two-Step Approach for the Stereodivergent Synthesis of 1,3-Diamines with Three Continuous Stereocenters.
Halli, Juliette; Bolte, Michael; Bats, Jan; Manolikakes, Georg; Organic letters 19 (2017) 674–677; doi:10.1021/acs.orglett.6b03841

data_1556015
_publ_section_title
;
 Modular Two-Step Approach for the Stereodivergent Synthesis of
 1,3-Diamines with Three Continuous Stereocenters.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              674
_journal_page_last               677
_journal_paper_doi               10.1021/acs.orglett.6b03841
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C26 H30 N2 O3'
_chemical_formula_sum            'C26 H30 N2 O3'
_chemical_formula_weight         418.52
_space_group_crystal_system      monoclinic
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_atom_sites_solution_hydrogens   mixed
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_cell_length_c                   22.5999(7)
_cell_measurement_reflns_used    26559
_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.07
_cell_volume                     4673.1(3)
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_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_min       -22
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_diffrn_reflns_limit_l_max       28
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_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.908
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
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_refine_diff_density_max         0.292
_refine_diff_density_min         -0.209
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_refine_ls_extinction_coef       0.0033(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0656P)^2^+3.7358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4388
_reflns_number_total             5029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            12c.cif
_cod_data_source_block           ma74
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1556015
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_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              96305
_shelx_hkl_checksum              83226