Mechanochemical reactivity inhibited, prohibited and reversed by liquid additives: examples from crystal-form screens
Arhangelskis, Mihails; Bučar, Dejan-Krešimir; Bordignon, Simone; Chierotti, Michele R.; Stratford, Samuel A.; Voinovich, Dario; Jones, William; Hasa, Dritan; Chemical Science 12 (2021) 3264–3269; doi:10.1039/D0SC05071G

data_1560124
_publ_section_title
;
 Mechanochemical reactivity inhibited, prohibited and reversed by liquid
 additives: examples from crystal-form screens
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3264
_journal_page_last               3269
_journal_paper_doi               10.1039/D0SC05071G
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H27 N2 O2, C2 H O4, 0.158(C4 H8 O2)'
_chemical_formula_sum            'C24.63 H29.26 N2 O6.32'
_chemical_formula_weight         454.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-20 deposited with the CCDC.	2020-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8855(2)
_cell_length_b                   6.32180(10)
_cell_length_c                   21.0313(3)
_cell_measurement_reflns_used    29449
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      72.3610
_cell_measurement_theta_min      4.3220
_cell_volume                     2293.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.636
_diffrn_reflns_theta_min         4.360
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             966.20
_exptl_crystal_face_perp_dist
;
  -3   -3   -9 0.1249
   5   -3    0 0.1842
   5    0   -1 0.0500
  -4   -3    5 0.1700
   4    3    4 0.1241
   0    0    1 0.0250
 -12    0    5 0.0489
   0    0   -1 0.0250
   4    0   -3 0.0528
;
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1916 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0518P)^2^+1.2181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                4366
_reflns_number_total             4462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05071g2.cif
_cod_data_source_block           EtOAc-solvate
_cod_depositor_comments
'Adding full bibliography for 1560122--1560124.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1560124
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              63153