Co-crystals of tetrahaloauric acid and 1,3,5-(methylacetamide)benzene-based tectons: consistent trapping of high energy molecular conformation
Shaffer, Cassandra C.; Oliver, Allen Grayson; Smith, B. D.; CrystEngComm  (2022) –; doi:10.1039/D2CE00463A

data_7244874
_publ_section_title
;
 Co-crystals of tetrahaloauric acid and
 1,3,5-(methylacetamide)benzene-based tectons: consistent trapping of high
 energy molecular conformation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00463A
_journal_year                    2022
_chemical_formula_moiety         'C21 H34 N3 O3, Au Br4'
_chemical_formula_sum            'C21 H34 Au Br4 N3 O3'
_chemical_formula_weight         893.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-14 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.800(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5789(11)
_cell_length_b                   17.0609(15)
_cell_length_c                   13.3931(12)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.32
_cell_volume                     2791.3(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            99093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.649
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.023
_exptl_absorpt_correction_T_max  0.6116
_exptl_absorpt_correction_T_min  0.2843
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / methanol / diethyl ether'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0185P)^2^+4.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6586
_reflns_number_total             8616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00463a2.cif
_cod_data_source_block           nd1904
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7244874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.230
_shelx_estimated_absorpt_t_max   0.444
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              11838
_shelx_hkl_checksum              92969