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_4135488
_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 Ag8 I2 N36, 6(C2 F6 N O4 S2), 1.4(C4 H10 O), 6.5(C2 H3 N)'
;
_chemical_formula_sum            'C223 H178.5 Ag8 F36 I2 N48.5 O25.5 S12'
_chemical_formula_weight         6131.11
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                80.5920(10)
_cell_angle_beta                 81.8190(10)
_cell_angle_gamma                79.0120(10)
_cell_formula_units_Z            2
_cell_length_a                   21.6420(3)
_cell_length_b                   24.0386(4)
_cell_length_c                   25.2054(4)
_cell_measurement_reflns_used    33259
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0021222029
_cell_measurement_theta_min      0.798405677124
_cell_volume                     12615.5(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.14.11-gcbedd378c-release'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.14.11-gcbedd378c-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.900-ga3de5862-dials-1.14 (Winter, G., 2010)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.981
_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_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            157389
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         0.799
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.975301320063
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.075: AIMLESS, version 0.7.4 : 13/12/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             6116
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.586
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3693
_refine_ls_number_reflns         50624
_refine_ls_number_restraints     7556
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25956
_reflns_number_total             50624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11905_si_002.cif
_cod_data_source_block           ctm426b_sq
_cod_original_formula_sum        'C223 H178.50 Ag8 F36 I2 N48.50 O25.50 S12'
_cod_database_code               4135488
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              56195
_shelx_hkl_checksum              70699
_shelx_fab_checksum              81625