Supramolecular intermediates in thermo-mechanochemical direct amidations
Stolar, Tomislav; Alić, Jasna; Talajić, Gregor; Cindro, Nikola; Rubčić, Mirta; Molcanov, Kresimir; Užarević, Krunoslav; Hernández, José G.; Chemical Communications  (2023) –; doi:10.1039/D3CC04448C

data_7132242
_publ_section_title
;
 Supramolecular intermediates in thermo-mechanochemical direct amidations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04448C
_journal_year                    2023
_chemical_formula_moiety
'C7 H9 N, 2(C7 H6 O2), 2(C7 H5 O2), 2(C7 H10 N)'
_chemical_formula_sum            'C49 H51 N3 O8'
_chemical_formula_weight         809.93
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-28T11:39:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-08-07 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   21.4268(3)
_cell_measurement_reflns_used    10223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.875
_cell_measurement_theta_min      4.125
_cell_volume                     2138.41(6)
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_computing_data_collection       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0624
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_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16943
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.876
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.569
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_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.69a (Rigaku Oxford Diffraction, 2022)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4564
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.7424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                4081
_reflns_number_total             4564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04448c2.cif
_cod_data_source_block           stolar_baptol-32_auto
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132242