Orthogonal, modular anion-cation and cation-anion self-assembly using pre-programmed anion binding sites.
Dhara, Ayan; Fadler, Rachel E.; Chen, Yusheng; Köttner, Laura A; Van Craen, David; Carta, Veronica; Flood, Amar H.; Chemical science 14 (2023) 2585–2595; doi:10.1039/d2sc05121d

data_1568455
_publ_section_title
;
 Orthogonal, modular anion-cation and cation-anion self-assembly using
 pre-programmed anion binding sites.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2585
_journal_page_last               2595
_journal_paper_doi               10.1039/d2sc05121d
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C31 H26 Au F N2 P, C2 F6 N O4 S2'
_chemical_formula_sum            'C33 H26 Au F7 N3 O4 P S2'
_chemical_formula_weight         953.62
_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
_audit_creation_date             2020-01-31
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-06-23 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                62.663(2)
_cell_angle_beta                 79.227(2)
_cell_angle_gamma                82.934(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6133(4)
_cell_length_b                   14.6051(6)
_cell_length_c                   15.5136(8)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.65
_cell_volume                     1701.53(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker VENTURE D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88532
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.516
_diffrn_reflns_theta_min         2.409
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.575
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0824 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.8622.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method
'vapor diffusion of dichloromethane into a diethyl ether solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.454
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     537
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+2.8537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9867
_reflns_number_total             10365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05121d2.cif
_cod_data_source_block           20022_0m
_cod_depositor_comments          'Adding full bibliography for 1568455.cif.'
_cod_database_code               1568455
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2-O4 \\sim S2-O3A
 with sigma of 0.02
 S3-O3 \\sim S3-O4A
 with sigma of 0.02
 S2-C1A \\sim S3-C33
 with sigma of 0.02
 F6A-C33 \\sim F5A-C33 \\sim F7A-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F2A) = Uanis(F3) = Uanis(F3A) = Uanis(F4A) = Uanis(F2)
Uanis(F6) = Uanis(F7A) = Uanis(F7) = Uanis(F5A) = Uanis(F5) = Uanis(F6A)
Uanis(O2) = Uanis(O2A)
Uanis(O1) = Uanis(O1A)
Uanis(O3) = Uanis(O3A)
Uanis(O4) = Uanis(O4A)
Uanis(C1A) = Uanis(C33)
Uanis(S4) = Uanis(S1)
Uanis(C32) = Uanis(C1B)
Uanis(S3) = Uanis(S2)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: S1(0.5) F7(0.5) C33(0.5) F2A(0.5) C32(0.5) F3(0.5) F5A(0.5)
 F4(0.5) F6(0.5) F6A(0.5) F4A(0.5) F7A(0.5) F3A(0.5) F5(0.5) F2(0.5) N4(0.5)
 N3(0.5) O2(0.5) O1(0.5) O1A(0.5) O2A(0.5) O4A(0.5) O3(0.5) O4(0.5) O3A(0.5)
 C1A(0.5) S4(0.5) C1B(0.5) S2(0.5) S3(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C31(H31), C16(H16), C25(H25), C1(H1), C17(H17), C19(H19), C21(H21),
 C6(H6), C27(H27), C8(H8), C9(H9), C22(H22), C24(H24), C30(H30), C12(H12),
 C23(H23), C18(H18), C29(H29), C28(H28), C3(H3), C2(H2), C11(H11)
6.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              33329
_shelx_hkl_checksum              68790
_olex2_submission_original_sample_id DVC310AD
_olex2_submission_special_instructions 'No special instructions were received'