A diversity-oriented synthesis of polyheterocycles via the cyclocondensation of azomethine imine
Ansari, Arshad J.; Pathare, Ramdas S.; Kumawat, Anita; Maurya, Antim K.; Verma, Sarika; Agnihotri, Vijai K.; Joshi, Rahul; Metre, Ramesh K.; Sharon, Ashoke; Pardasani, R. T.; Sawant, Devesh M.; New Journal of Chemistry 43 (2019) 13721–; doi:10.1039/C9NJ02874A

data_7058715
_publ_section_title
;
 A diversity-oriented synthesis of polyheterocycles via the
 cyclocondensation of azomethine imine
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13721
_journal_paper_doi               10.1039/C9NJ02874A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '2(C28 H30 Br N5 O4 S)'
_chemical_formula_sum            'C28 H30 Br N5 O4 S'
_chemical_formula_weight         612.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-12-02 deposited with the CCDC.    2019-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                82.601(2)
_cell_angle_beta                 89.156(2)
_cell_angle_gamma                78.132(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1312(14)
_cell_length_b                   12.9663(17)
_cell_length_c                   19.980(3)
_cell_measurement_reflns_used    8635
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.89
_cell_volume                     2798.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21705
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.03
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.587
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1666 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.6795.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.588
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.365
_refine_ls_extinction_coef       0.047(3)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         12453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                9791
_reflns_number_total             12453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj02874a2.cif
_cod_data_source_block           mcr_a122_030_07_07_2017_0m
_cod_depositor_comments
'Adding full bibliography for 7058715--7058716.cif.'
_cod_original_cell_volume        2798.4(6)
_cod_database_code               7058715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5A), C12(H12), C38(H38), C40(H40)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), N11(H11A), N5(H5), C3(H3), C2AA(H2AA), C7(H7), C1AA(H1AA),
 C9(H9), C10(H10), C11(H11), C15(H15), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C32(H32), C33(H33), C36(H36), C42(H42), C43(H43), C45(H45), C46(H46),
  C53(H53), C54(H54)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C35(H35A,H35B,H35C), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'