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_7244873
_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         '4(C19 H28 N3 O3), 4(Au Br4), C4 H10 O'
_chemical_formula_sum            'C76 H122 Au4 Br16 N12 O13'
_chemical_formula_weight         3478.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                71.990(5)
_cell_angle_beta                 82.849(5)
_cell_angle_gamma                74.244(4)
_cell_formula_units_Z            1
_cell_length_a                   11.433(3)
_cell_length_b                   14.321(4)
_cell_length_c                   19.606(6)
_cell_measurement_reflns_used    3026
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.43
_cell_measurement_theta_min      2.28
_cell_volume                     2935.3(14)
_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, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON-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  0.0973
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29675
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         1.093
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.480
_exptl_absorpt_correction_T_max  08718
_exptl_absorpt_correction_T_min  0.4190
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description       blade
_exptl_crystal_F_000             1642
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / methanol / diethyl ether'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.016
_refine_diff_density_max         5.955
_refine_diff_density_min         -3.123
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1096P)^2^+127.0232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5556
_reflns_number_total             8423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00463a2.cif
_cod_data_source_block           nd1854_sq
_cod_original_cell_volume        2935.2(15)
_cod_database_code               7244873
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.328
_shelx_estimated_absorpt_t_max   0.850
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              86051
_shelx_hkl_checksum              20532
_shelx_fab_checksum              60248