Catalyst-Free Synthesis of Aryl Diamines via a Three-Step Reaction Process.
Bulut, Safak; Queen, Wendy L.; The Journal of organic chemistry 83 (2018) 3806–3818; doi:10.1021/acs.joc.8b00151

data_4035500
_publ_section_title
;
 Catalyst-Free Synthesis of Aryl Diamines via a Three-Step Reaction
 Process.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3806
_journal_page_last               3818
_journal_paper_doi               10.1021/acs.joc.8b00151
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C42 H62 N4 O11'
_chemical_formula_weight         798.95
_chemical_name_common            'CCDC 1540294_Compound 5_SB22_fromTHF'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.060(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.222(8)
_cell_length_b                   8.278(6)
_cell_length_c                   18.419(10)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      43.551
_cell_measurement_theta_min      4.579
_cell_volume                     1956(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  Venture
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22161
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        21.871
_diffrn_reflns_theta_max         21.871
_diffrn_reflns_theta_min         2.168
_exptl_absorpt_coefficient_mu    0.098
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0405
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1979
_reflns_number_total             2288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00151_si_002.cif
_cod_data_source_block           SB22_fromTHF
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4035500
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              64459
_shelx_hkl_checksum              49461