Establishing Parameters for Resonant Acoustic Mixing (RAM) Chemistry using Buchwald-Hartwig Amination as a Model
Gonnet, Lori; Lennox, Cameron B.; Borchers, Tristan H.; Askari, Mohammad; Wahrhaftig-Lewis, Alexander; Koenig, Stefan G.; Nagapudi, Karthik; Friščić, Tomislav; Green Chemistry  (2026) –; doi:10.1039/D6GC00784H

data_7251670
_publ_section_title
;
 Establishing Parameters for Resonant Acoustic Mixing (RAM) Chemistry
 using Buchwald-Hartwig Amination as a Model
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/D6GC00784H
_journal_year                    2026
_chemical_formula_moiety         'C32 H26 F6 N14 Nd2 O16'
_chemical_formula_sum            'C32 H26 F6 N14 Nd2 O16'
_chemical_formula_weight         1265.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2kmmpj
_audit_creation_date             2024-06-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2024-07-21 deposited with the CCDC.	2026-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.465(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0681(9)
_cell_length_b                   12.9657(4)
_cell_length_c                   14.4992(6)
_cell_measurement_reflns_used    8712
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      29.5270
_cell_measurement_theta_min      1.4540
_cell_volume                     3998.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -41.00  67.00   0.50    1.27    --  -11.46  48.00 -16.00  216
  2  \w    -11.00  32.00   0.50    1.27    --  -11.46 -99.00  60.00   86
  3  \w      7.00  34.00   0.50    1.27    --  -11.46 -99.00   0.00   54
  4  \w     -9.00  16.00   0.50    1.27    --  -11.46 -99.00-150.00   50
  5  \w    -83.00  -9.00   0.50    1.27    --  -11.46 -48.00-164.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0332640000
_diffrn_orient_matrix_UB_12      -0.0000055000
_diffrn_orient_matrix_UB_13      0.0090157000
_diffrn_orient_matrix_UB_21      0.0025233000
_diffrn_orient_matrix_UB_22      -0.0321019000
_diffrn_orient_matrix_UB_23      0.0404148000
_diffrn_orient_matrix_UB_31      -0.0018030000
_diffrn_orient_matrix_UB_32      -0.0442777000
_diffrn_orient_matrix_UB_33      -0.0292673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11245
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+28.6643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                3168
_reflns_number_total             3526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d6gc00784h2.cif
_cod_data_source_block           jxh2-3nd-2-100k
_cod_database_code               7251670
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O8-H8A
 0.87 with sigma of 0.01
 Nd1-H8A
 2.95239 with sigma of 0.02
 C16-H8A
 1.927037 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14), N3(H3A)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.153
_oxdiff_exptl_absorpt_empirical_full_min 0.506