Post-Ugi Transformations for the Access to Pyrrolobenzodiazepine Scaffolds with Different Degrees of Unsaturation.
Pertejo, Pablo; Carreira-Barral, Israel; Peña-Calleja, Pablo; Quesada, Roberto; García-Valverde, María; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b02995

data_4037844
_publ_section_title
;
 Post-Ugi Transformations for the Access to Pyrrolobenzodiazepine
 Scaffolds with Different Degrees of Unsaturation.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02995
_journal_year                    2020
_chemical_formula_moiety         'C26 H28 Cl N3 O3, C H Cl3'
_chemical_formula_sum            'C27 H29 Cl4 N3 O3'
_chemical_formula_weight         585.33
_chemical_name_systematic        12i
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
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_cell_angle_beta                 102.591(2)
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_cell_formula_units_Z            2
_cell_length_a                   10.1498(15)
_cell_length_b                   11.4460(16)
_cell_length_c                   12.8648(18)
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_cell_measurement_temperature    100(2)
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_cell_volume                     1344.1(3)
_computing_cell_refinement       'Bruker SMART'
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_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
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_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_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_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.908
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_diffrn_reflns_theta_min         1.751
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.300
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_refine_ls_number_reflns         6020
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_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4173
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02995_si_002.cif
_cod_data_source_block           12i
_cod_database_code               4037844
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              71321
_shelx_hkl_checksum              35185