Microwave-assisted [3 + 2] cycloaddition reactions of dicyanoepoxides with benzylidene Meldrum's acids.
Lotfi Nosood, Yazdanbakhsh; Fattahi Ghahnavieh, Negin; Takallou, Ahmad; Rostami, Ali; Ebrahimi, Amirhossein; Anwar, Muhammad U.; Al-Harrasi, Ahmed; Organic & biomolecular chemistry 23 (2025) 4084–4089; doi:10.1039/d4ob01702a

data_7160345
_publ_section_title
;
 Microwave-assisted [3 + 2] cycloaddition reactions of dicyanoepoxides
 with benzylidene Meldrum's acids.
;
_journal_issue                   17
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4084
_journal_page_last               4089
_journal_paper_doi               10.1039/d4ob01702a
_journal_volume                  23
_journal_year                    2025
_chemical_formula_sum            'C24 H19 Cl N2 O6'
_chemical_formula_weight         466.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
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_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V135 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-10-13 deposited with the CCDC.	2025-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_b                   23.8348(13)
_cell_length_c                   12.1335(7)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.2535
_cell_measurement_theta_min      2.6415
_cell_volume                     2406.4(2)
_computing_cell_refinement       'SAINT V8.40B'
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'Bruker BIS V6.2.16/2021-10-23 and APEX4 2022.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
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_diffrn_ambient_temperature      296(2)
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_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_diffrn_measurement_method       '\w and \f scans'
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_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41089
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0422P)^2^+3.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3322
_reflns_number_total             4905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01702a2.cif
_cod_data_source_block           LSR_Yazdan_R1_0m_a
_cod_depositor_comments
'Adding full bibliography for 7160345--7160346.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7160345
_shelx_shelxl_version_number     2019/1
_diffrn_measurement_ambient_temperature_device_make '296 K'
_shelx_res_checksum              65939