Synthesis and ethylene-promoted metathesis of adducts of tandem [4+2]/[4+2] cycloaddition between bis-furyl dienes and maleic acid derivatives
Kvyatkovskaya, Elizaveta A.; Epifanova, Polina P.; Nikitina, Eugeniya V.; Senin, Aleksey A.; Khrustalev, Victor N.; Polyanskii, Kirill B.; Zubkov, Fedor I.; New Journal of Chemistry 45 (2021) 3400–3407; doi:10.1039/D0NJ04528D

data_7060347
_publ_section_title
;
 Synthesis and ethylene-promoted metathesis of adducts of tandem
 [4+2]/[4+2] cycloaddition between bis-furyl dienes and maleic acid
 derivatives
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3400
_journal_page_last               3407
_journal_paper_doi               10.1039/D0NJ04528D
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H15 N O5'
_chemical_formula_sum            'C15 H15 N O5'
_chemical_formula_weight         289.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-08-30 deposited with the CCDC.	2021-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.625(3)
_cell_length_b                   7.2251(14)
_cell_length_c                   10.625(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.3
_cell_volume                     1275.4(4)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_unetI/netI     0.1698
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11008
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         35.996
_diffrn_reflns_theta_min         3.347
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 1234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_coef       0.048(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.1082
_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^)+7.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2459
_refine_ls_wR_factor_ref         0.2632
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                3252
_reflns_number_total             4262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04528d2.cif
_cod_data_source_block           4e
_cod_depositor_comments
'Adding full bibliography for 7060344--7060348.cif.'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7060347
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2013-4
_shelx_res_checksum              41351