Palladium-catalyzed regio- and stereoselective access to allyl ureas/carbamates: facile synthesis of imidazolidinones and oxazepinones.
Taily, Irshad Maajid; Saha, Debarshi; Banerjee, Prabal; Organic & biomolecular chemistry 18 (2020) 6564–6570; doi:10.1039/d0ob01514h

data_7157645
_publ_section_title
;
 Palladium-catalyzed regio- and stereoselective access to allyl
 ureas/carbamates: facile synthesis of imidazolidinones and oxazepinones.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6564
_journal_page_last               6570
_journal_paper_doi               10.1039/d0ob01514h
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C12 H16 N2 O4'
_chemical_formula_sum            'C12 H16 N2 O4'
_chemical_formula_weight         252.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-20 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.621(2)
_cell_length_b                   8.003(2)
_cell_length_c                   33.196(9)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.5
_cell_volume                     2556.0(11)
_computing_cell_refinement       'SAINT V8.38A (BRUKER AXS INC., 2017)'
_computing_data_collection       'APEX3 INC.,BRUKER SOFTWARE PACKAGE'
_computing_data_reduction        'SAINT V8.38A (BRUKER AXS INC., 2017)'
_computing_molecular_graphics    'ORTEP3 MERCURY AND PLATON'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (SHELDRICK,2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'BRUKER D8 VENTURE, PHOTON 200'
_diffrn_measurement_method       'PHI AND OMEGA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            16285
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.151
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'FINE FOCUSED SEALED TUBE'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      1.3
_exptl_crystal_density_method    'NOT MEASURED'
_exptl_crystal_description       'BLOCK TYPE'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.245
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6018
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1220 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0658P)^2^+1.5494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.806
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                3495
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01514h2.cif
_cod_data_source_block           shelx
_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/RSC/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 

 Adding full bibliography for 7157645--7157646.cif.

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2555.8(11)
_cod_original_formula_moiety     'C24 H32 N4 O8'
_cod_original_formula_sum        'C24 H32 N4 O8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     504.53
_cod_database_code               7157645
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              7756
_shelx_hkl_checksum              26265