Solid-phase Synthesis of Hybrid 2,5-Diketopiperazines Using Acylhydrazide, Carbazate, Semicarbazide, Amino Acid and Primary Amine Submonomers.
Rahim, Abdur; Sahariah, Biswajit; Baruah, Kalpita; Deka, Jugal Kishore Rai; Sarma, Bani Kanta; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b02083

data_4037904
_publ_section_title
;
 Solid-phase Synthesis of Hybrid 2,5-Diketopiperazines Using
 Acylhydrazide, Carbazate, Semicarbazide, Amino Acid and Primary Amine
 Submonomers.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02083
_journal_year                    2020
_chemical_formula_moiety         'C20 H20 N4 O6'
_chemical_formula_sum            'C20 H20 N4 O6'
_chemical_formula_weight         412.40
_chemical_name_systematic
'dibenzyl (2,5-dioxopiperazine-1,4-diyl)dicarbamate'
_space_group_crystal_system      monoclinic
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-12-30 deposited with the CCDC.	2019-12-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.0913(9)
_cell_length_b                   5.7683(3)
_cell_length_c                   8.6111(3)
_cell_measurement_reflns_used    6706
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      3.10
_cell_volume                     980.49(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15073
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         2.063
_diffrn_source                   X-ray
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0414
_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^+0.4952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1717
_reflns_number_total             1998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02083_si_002.cif
_cod_data_source_block           Comp32_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        980.48(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4037904
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              7332
_shelx_hkl_checksum              14345