Selective Anion Binding Drives the Formation of AgI8L6 and AgI12L6 Six-Stranded Helicates
McTernan, Charlie T.; Ronson, Tanya K.; Nitschke, Jonathan R.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11905

data_4135489
_publ_section_title
;
 Selective Anion Binding Drives the Formation of AgI8L6 and AgI12L6
 Six-Stranded Helicates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11905
_journal_year                    2020
_chemical_formula_moiety
;
'C192 H144 Ag12 N36 O16 S4, 4(B F4), 2(C4 H10 O), 10.5(C2 H3 N), 4.5(H2 O)'
;
_chemical_formula_sum            'C221 H204.5 Ag12 B4 F16 N46.5 O22.5 S4'
_chemical_formula_weight         5641.72
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.97750(10)
_cell_length_b                   23.97750(10)
_cell_length_c                   70.6392(3)
_cell_measurement_reflns_used    58901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.4875688208
_cell_measurement_theta_min      1.09828302322
_cell_volume                     35171.0(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 2.1.4-ga615ced2f-release'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
DIALS 2.1.4-ga615ced2f-release (Winter, G. et al., 2018)
XIA2 0.6.380-g0f31cbd4-dials-2.1 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       108
_diffrn_reflns_limit_l_min       -108
_diffrn_reflns_number            183793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         31.999
_diffrn_reflns_theta_min         1.103
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9813060754116014
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 2.1.4-ga615ced2f-release
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       prism
_exptl_crystal_F_000             16968
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.437
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         29726
_refine_ls_number_restraints     1736
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1077P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21845
_reflns_number_total             29726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11905_si_003.cif
_cod_data_source_block           ctm5502_sq
_cod_original_cell_volume        35170.9(3)
_cod_original_formula_sum        'C221 H204.50 Ag12 B4 F16 N46.50 O22.50 S4'
_cod_database_code               4135489
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              60587
_shelx_hkl_checksum              63349
_shelx_fab_checksum              34152