Rapid and facile solvent-free mechanosynthesis in a cell lysis mill: preparation and mechanochemical complexation of aminobenzoquinones
Fang, Yuan; Salamé, Nadime; Woo, Simon; Bohle, D. Scott; Friščić, Tomislav; Cuccia, Louis A.; CrystEngComm 16 (2014) 7180–; doi:10.1039/C4CE00328D

data_7216617
_publ_section_title
;
 Rapid and facile solvent-free mechanosynthesis in a cell lysis mill:
 preparation and mechanochemical complexation of aminobenzoquinones
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7180
_journal_paper_doi               10.1039/C4CE00328D
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C31 H58 N2 O3'
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                94.6260(10)
_cell_angle_beta                 98.4530(10)
_cell_angle_gamma                101.5280(10)
_cell_formula_units_Z            2
_cell_length_a                   6.6943(6)
_cell_length_b                   15.4475(15)
_cell_length_c                   15.5647(15)
_cell_measurement_temperature    100(2)
_cell_volume                     1549.9(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.250
_diffrn_reflns_theta_min         1.331
_exptl_absorpt_coefficient_mu    0.068
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_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0858P)^2^+1.4741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5373
_reflns_number_total             7128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00328d2.cif
_cod_data_source_block           lc10_0m_a
_cod_depositor_comments          'Adding full bibliography for 7216617.cif.'
_cod_database_code               7216617
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014-3
_shelx_res_checksum              6919