C1 functionalization of imidazo heterocycles via carbon dioxide fixation
Neochoritis, Constantinos G.; Fragkiadakis , Michael; Anastasiou, Paraskevi-Kleio; Volyrakis, Ioannis; Pantousas, Apostolos; Stoumpos, Constantinos C.; Chemical Communications  (2023) –; doi:10.1039/D3CC04597H

data_7132340
_publ_section_title
;
 C1 functionalization of imidazo heterocycles via carbon dioxide fixation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04597H
_journal_year                    2023
_chemical_formula_moiety         'C16 H16 Cl N3 O'
_chemical_formula_sum            'C16 H16 Cl N3 O'
_chemical_formula_weight         301.77
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-13 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                96.538(13)
_cell_angle_beta                 96.978(11)
_cell_angle_gamma                90.269(13)
_cell_formula_units_Z            4
_cell_length_a                   7.804(3)
_cell_length_b                   9.955(4)
_cell_length_c                   19.163(7)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      4.304
_cell_volume                     1467.9(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.3286
_diffrn_reflns_av_unetI/netI     0.1814
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63756
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.060
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4945
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       'elongated needle'
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.029
_exptl_transmission_factor_max   0.9920
_exptl_transmission_factor_min   0.9480
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.2790
_refine_ls_R_factor_gt           0.1487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3815
_refine_ls_wR_factor_ref         0.4528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2157
_reflns_number_total             5791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04597h2.cif
_cod_data_source_block           4
_cod_original_cell_volume        1467.8(9)
_cod_database_code               7132340
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              83922
_shelx_hkl_checksum              1981