Crystal Transformation from the Incorporation of Coordinate Bonds into a Hydrogen-Bonded Network Yields Robust Free-Standing Supramolecular Membranes.
Meng, Peng; Brock, Aidan; Xu, Yanan; Han, Chenhui; Chen, Su; Yan, Cheng; McMurtrie, John; Xu, Jingsan; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11336

data_4133870
_publ_section_title
;
 Crystal Transformation from the Incorporation of Coordinate Bonds into a
 Hydrogen-Bonded Network Yields Robust Free-Standing Supramolecular
 Membranes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11336
_journal_year                    2019
_chemical_formula_moiety         '0.5(C12 H14 Ag4 N18 O6)'
_chemical_formula_sum            'C6 H7 Ag2 N9 O3'
_chemical_formula_weight         468.95
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                68.910(3)
_cell_angle_beta                 85.125(2)
_cell_angle_gamma                84.854(2)
_cell_formula_units_Z            4
_cell_length_a                   3.471
_cell_length_b                   19.3414(6)
_cell_length_c                   20.4117(8)
_cell_measurement_reflns_used    2736
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.8170
_cell_measurement_theta_min      2.4930
_cell_volume                     1271.33(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.699
_diffrn_measured_fraction_theta_max 0.699
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 360.00   0.10    0.01   0.00   0.00   0.00    --  3600
;
_diffrn_measurement_device       'Eiger 16 X M'
_diffrn_measurement_device_type  'Eiger 16 X M'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.699
_diffrn_reflns_Laue_measured_fraction_max 0.699
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6069
_diffrn_reflns_point_group_measured_fraction_full 0.351
_diffrn_reflns_point_group_measured_fraction_max 0.351
_diffrn_reflns_theta_full        25.126
_diffrn_reflns_theta_max         25.126
_diffrn_reflns_theta_min         1.813
_exptl_absorpt_coefficient_mu    3.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.450
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.624
_refine_diff_density_min         -2.174
_refine_diff_density_rms         0.467
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.56(6)
_refine_ls_extinction_coef       0.013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         6069
_refine_ls_number_restraints     1089
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0935
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.2718
_reflns_Friedel_coverage         0.006
_reflns_Friedel_fraction_full    0.004
_reflns_Friedel_fraction_max     0.004
_reflns_number_gt                4430
_reflns_number_total             6069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11336_si_002.cif
_cod_data_source_block           twin2_twin1_hklf4_sq
_cod_original_cell_volume        1271.29(7)
_cod_database_code               4133870
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.516(3)
 0.484(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(N25) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(Ag1)
\\sim Ueq, Uanis(Ag7) \\sim Ueq, Uanis(Ag2) \\sim Ueq, Uanis(Ag3) \\sim Ueq,
Uanis(Ag6) \\sim Ueq, Uanis(Ag8) \\sim Ueq, Uanis(Ag5) \\sim Ueq, Uanis(Ag4)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N31) \\sim Ueq, Uanis(N33) \\sim Ueq,
Uanis(N24) \\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N35) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(N19) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N8) \\sim Ueq,
Uanis(N28) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(N20) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N23) \\sim Ueq,
Uanis(N27) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N32)
\\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N21) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(C11) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(N16) \\sim Ueq,
Uanis(N9) \\sim Ueq, Uanis(N30) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(N34)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N29) \\sim Ueq, Uanis(N15) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N36)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N10) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N34) = Uanis(C24) = Uanis(N36) = Uanis(N35) = Uanis(O10) = Uanis(O11) =
Uanis(O12)
Uanis(C4) = Uanis(N4)
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.a Fitted hexagon refined as free rotating group:
 N25(C18,N27,C17,N26,C16), N9(C6,N7,C5,N5,C4), C10(N13,C12,N17,C11,N15),
 N10(C9,N12,C8,N11,C7)
5.b X=CH2 refined with riding coordinates:
 N20(H20A,H20B), N8(H8A,H8B), N29(H29A,H29B), N18(H18A,H18B), N16(H16A,H16B),
 N6(H6A,H6B), N14(H14A,H14B), N4(H4A,H4B), N22(H22A,H22B), N24(H24A,H24B),
 N33(H33A,H33B), N31(H31A,H31B)
5.c Idealised tetrahedral OH refined as rotating group:
 O12(H12), O9(H9), O6(H6), O3(H3)
;
_shelx_res_checksum              83772
_shelx_hkl_checksum              71691
_shelx_fab_checksum              46849
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_twin_special_details
;
Component 2 rotated by -179.9916\% 
 around [0.00 0.68 0.73] (reciprocal) or [-0.58 0.58 0.58] (direct)
;