Macrocyclic Receptor for Precious Gold, Platinum, or Palladium Coordination Complexes.
Liu, Wenqi; Oliver, Allen G.; Smith, Bradley D.; Journal of the American Chemical Society 140 (2018) 6810–6813; doi:10.1021/jacs.8b04155

data_4132471
_publ_section_title
;
 Macrocyclic Receptor for Precious Gold, Platinum, or Palladium
 Coordination Complexes.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6810
_journal_page_last               6813
_journal_paper_doi               10.1021/jacs.8b04155
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C48 H60 N4 O4, Au Br4, C16 H36 N, 3(C H Cl3)'
_chemical_formula_sum            'C67 H99 Au Br4 Cl9 N5 O4'
_chemical_formula_weight         1874.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.768(3)
_cell_length_b                   15.419(2)
_cell_length_c                   23.157(3)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.39
_cell_volume                     7772.4(18)
_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-2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (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 0.993
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            175496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_min         1.587
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_T_max  0.7739
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.869
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 6303 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         19343
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+36.7691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                15111
_reflns_number_total             19343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04155_si_006.cif
_cod_data_source_block           nd1720
_cod_original_cell_volume        7772.2(19)
_cod_database_code               4132471
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.708
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              76913
_shelx_hkl_checksum              3669