Resonant acoustic mixing (RAM) for efficient mechanoredox catalysis without grinding or impact media.
Effaty, Farshid; Gonnet, Lori; Koenig, Stefan G.; Nagapudi, Karthik; Ottenwaelder, Xavier; Friščić, Tomislav; Chemical communications (Cambridge, England) 59 (2023) 1010–1013; doi:10.1039/d2cc06013b

data_7131102
_publ_section_title
;
 Resonant acoustic mixing (RAM) for efficient mechanoredox catalysis
 without grinding or impact media.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1010
_journal_page_last               1013
_journal_paper_doi               10.1039/d2cc06013b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C15 H22 N2 O3'
_chemical_formula_sum            'C15 H22 N2 O3'
_chemical_formula_weight         278.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2d0r06
_audit_creation_date             2022-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2022-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   17.1295(4)
_cell_length_b                   17.2313(4)
_cell_length_c                   42.1825(11)
_cell_measurement_reflns_used    17385
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      72.394
_cell_measurement_theta_min      2.096
_cell_volume                     12442.4(5)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '/w and /f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            119759
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.394
_diffrn_reflns_theta_min         2.096
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.7287
_exptl_absorpt_correction_T_min  0.6367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1544 before and 0.1012 after correction.
The Ratio of minimum to maximum transmission is 0.8737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexanes'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.3(4)
_refine_ls_extinction_coef       0.00247(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         24094
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+7.0526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2434
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                17385
_reflns_number_total             24094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06013b2.cif
_cod_data_source_block           s4_a
_cod_depositor_comments          'Adding full bibliography for 7131102.cif.'
_cod_database_code               7131102
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7(4)
 0.3(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C12F(H12A,H12B), C14F(H14A,H14B), C13F(H13A,H13B), C14C(H14C,H14D), C15C(H15A,
 H15B), C13C(H13C,H13D), C14J(H14E,H14F), C13J(H13E,H13F), C15J(H15C,H15D),
 C14G(H14G,H14H), C15G(H15E,H15F), C13G(H13G,H13H), C13D(H13I,H13J), C14D(H14I,
 H14J), C15D(H15G,H15H), C15A(H15I,H15J), C13A(H13K,H13L), C14A(H14K,H14L),
 C17E(H17S,H17T), C16E(H16D,H16E), C13E(H13M,H13N), C14B(H14M,H14N), C13B(H13O,
 H13P), C15B(H15K,H15L)
3.b Aromatic/amide H refined with riding coordinates:
 C3F(H3F), C5F(H5F), C01R(H01R), C2F(H2F), C5C(H5C), C2C(H2C), C3C(H3C),
 C6C(H6C), C2J(H2J), C3J(H3J), C6J(H6J), C5J(H5J), C3G(H3G), C2G(H2G), C6G(H6G),
  C5G(H5G), C3D(H3D), C2D(H2D), C6D(H6D), C5D(H5D), C5A(H5A), C3A(H3A),
 C2A(H2A), C6A(H6A), C2E(H2E), C6E(H6E), C3E(H3E), C5E(H5E), C5B(H5B), C6B(H6B),
  C3B(H3B), C2B(H2B)
3.c Idealised Me refined as rotating group:
 C19F(H19A,H19B,H19C), C16F(H16A,H16B,H16C), C17F(H17A,H17B,H17C), C18F(H18A,
 H18B,H18C), C17C(H17D,H17E,H17F), C20C(H20A,H20B,H20C), C18C(H18D,H18E,H18F),
 C19C(H19D,H19E,H19F), C21J(H21A,H21B,H21C), C18J(H18G,H18H,H18I), C19J(H19G,
 H19H,H19I), C17J(H17G,H17H,H17I), C19G(H19J,H19K,H19L), C21G(H21D,H21E,H21F),
 C18G(H18J,H18K,H18L), C17G(H17J,H17K,H17L), C20G(H20D,H20E,H20F), C20D(H20G,
 H20H,H20I), C19D(H19M,H19N,H19O), C17D(H17M,H17N,H17O), C19A(H19P,H19Q,H19R),
 C17A(H17P,H17Q,H17R), C18A(H18M,H18N,H18O), C20A(H20J,H20K,H20L), C21E(H21G,
 H21H,H21I), C20E(H20M,H20N,H20O), C19E(H19S,H19T,H19U), C22E(H22A,H22B,H22C),
 C18B(H18P,H18Q,H18R), C20B(H20P,H20Q,H20R), C16B(H16F,H16G,H16H), C19B(H19V,
 H19W,H19X)
;
_shelx_res_checksum              78543
_shelx_hkl_checksum              29013
_shelx_fab_checksum              96405
_olex2_submission_special_instructions 'No special instructions were received'