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_4132470
_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, 2(C2 H6 O S), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C52.5 H73 Cl N4 O6 S2'
_chemical_formula_weight         955.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c 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                   17.2894(3)
_cell_length_b                   11.2213(2)
_cell_length_c                   27.5815(7)
_cell_measurement_reflns_used    5357
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.42
_cell_measurement_theta_min      3.20
_cell_volume                     5351.07(19)
_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 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.256
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8447
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       plate
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         10380
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0816
_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^)+(0.1428P)^2^+1.0030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2057
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8996
_reflns_number_total             10380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04155_si_004.cif
_cod_data_source_block           nd1715
_cod_original_cell_volume        5351.08(19)
_cod_original_formula_sum        'C52.50 H73 Cl N4 O6 S2'
_cod_database_code               4132470
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.630
_shelx_estimated_absorpt_t_max   0.972
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelx_res_checksum              3659
_shelx_hkl_checksum              78379