Enal-azomethine ylides: application in the synthesis of functionalized pyrroles.
Mandal, Pratap Kumar; Patel, Sandeep; Katukojvala, Sreenivas; Organic & biomolecular chemistry 22 (2024) 5734–5738; doi:10.1039/d4ob00859f

data_7160008
_publ_section_title
;
 Enal-azomethine ylides: application in the synthesis of functionalized
 pyrroles.
;
_journal_issue                   28
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5734
_journal_page_last               5738
_journal_paper_doi               10.1039/d4ob00859f
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C21 H13 Cl2 N O2'
_chemical_formula_sum            'C21 H13 Cl2 N O2'
_chemical_formula_weight         383.22
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-17 deposited with the CCDC.	2024-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.776(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.445(3)
_cell_length_b                   19.168(6)
_cell_length_c                   9.550(3)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.35
_cell_volume                     1775.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            33909
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.344
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.382
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             784
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0484
_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^)+(0.1048P)^2^+0.2062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3363
_reflns_number_total             4385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob00859f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7160008.cif.'
_cod_original_cell_volume        1775.7(9)
_cod_database_code               7160008
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H00C), C17(H00D), C00D(H00E), C4(H00F), C19(H00G), C18(H00J), C14(H00M),
 C10(H00N), C13(H00O), C11(H00P)
2.c :
 C1(H1)
;
_shelx_res_checksum              75755
_olex2_submission_special_instructions 'No special instructions were received'