Metal-Free [2 + 2 + 2] Cycloaddition of Ynamides with Nitriles to Construct 2,4-Diaminopyridines.
Zhang, Jingyi; Zhang, Qingshuang; Xia, Biao; Wu, Jie; Wang, Xiao-Na; Chang, Junbiao; Organic letters 18 (2016) 3390–3393; doi:10.1021/acs.orglett.6b01546

data_1555602
_publ_section_title
;
 Metal-Free [2 + 2 + 2] Cycloaddition of Ynamides with Nitriles to
 Construct 2,4-Diaminopyridines.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3390
_journal_page_last               3393
_journal_paper_doi               10.1021/acs.orglett.6b01546
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C41 H39 N3 O4 S2'
_chemical_formula_weight         701.87
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.9150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.8089(12)
_cell_length_b                   9.9944(3)
_cell_length_c                   20.8313(7)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      68.35
_cell_measurement_theta_min      2.66
_cell_volume                     7496.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31762
_diffrn_reflns_theta_full        68.47
_diffrn_reflns_theta_max         68.47
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.7677
_exptl_absorpt_correction_T_min  0.7455
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.764
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1795P)^2^+5.9346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                5413
_reflns_number_total             6845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b01546_si_003.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               1555602