Metal-free multicomponent synthesis of novel macrocyclic tetrathiadienes with cyano and amino groups
Akhmadiev, Nail S.; Mescheryakova, Ekaterina S.; Akhmetova, Vnira R.; Ibragimov, Askhat G.; RSC Advances 11 (2021) 18768–18775; doi:10.1039/D1RA02616J

data_7242924
_publ_section_title
;
 Metal-free multicomponent synthesis of novel macrocyclic tetrathiadienes
 with cyano and amino groups
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              18768
_journal_page_last               18775
_journal_paper_doi               10.1039/D1RA02616J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C10 H5 F N2'
_chemical_formula_sum            'C10 H5 F N2'
_chemical_formula_weight         172.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2020-12-23
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2021-02-20 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                107.194(8)
_cell_angle_beta                 99.036(9)
_cell_angle_gamma                102.848(8)
_cell_formula_units_Z            2
_cell_length_a                   6.9541(7)
_cell_length_b                   7.3664(5)
_cell_length_c                   9.1492(10)
_cell_measurement_reflns_used    1411
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.0147
_cell_measurement_theta_min      2.3951
_cell_volume                     423.86(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1709
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -92.00  -12.00   1.0000    5.2300
omega____ theta____ kappa____ phi______ frames
    -      -23.6098  -57.0000  -30.0000 80

  2 omega  -97.00   13.00   1.0000    5.2300
omega____ theta____ kappa____ phi______ frames
    -      -23.6098  -19.0000   30.0000 110

  3 omega  -71.00  -33.00   1.0000    5.2300
omega____ theta____ kappa____ phi______ frames
    -      -23.6098  115.0000   58.0000 38

  4 omega  -42.00   36.00   1.0000    5.2300
omega____ theta____ kappa____ phi______ frames
    -      -23.6098   57.0000 -150.0000 78

  5 omega    5.00   76.00   1.0000    5.2300
omega____ theta____ kappa____ phi______ frames
    -       24.5473 -115.0000  -58.0000 71
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0428398000
_diffrn_orient_matrix_UB_12      0.0182415000
_diffrn_orient_matrix_UB_13      0.0804229000
_diffrn_orient_matrix_UB_21      -0.0955171000
_diffrn_orient_matrix_UB_22      0.0020252000
_diffrn_orient_matrix_UB_23      0.0174240000
_diffrn_orient_matrix_UB_31      -0.0254958000
_diffrn_orient_matrix_UB_32      -0.1035371000
_diffrn_orient_matrix_UB_33      -0.0146284000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3675
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.084
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       prizm
_exptl_crystal_F_000             176.0
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.17(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0623P)^2^+0.0418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1863
_reflns_number_total             2396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02616j2.cif
_cod_data_source_block           ans-257
_cod_original_cell_volume        423.86(7)
_cod_database_code               7242924
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
;