Arene guest selectivity and pore flexibility in a metal-organic framework with semi-fluorinated channel walls
Rebecca Smith; Inigo J. Vitorica-Yrezabal; Adrian Hill; Lee Brammer; Philosophical Transactions of the Royal Society A 375 (2017) 1–16; doi:10.1098/rsta.2016.0031

data_1548413
_publ_section_title
;
 Arene guest selectivity and pore flexibility in a metal-organic framework
 with semi-fluorinated channel walls
;
_journal_name_full
'Philosophical Transactions of the Royal Society A'
_journal_page_first              1
_journal_page_last               16
_journal_paper_doi               10.1098/rsta.2016.0031
_journal_volume                  375
_journal_year                    2017
_chemical_formula_moiety         'C96 H96 Ag16 F32 N16 O32, 13(C O)'
_chemical_formula_sum            'C109 H96 Ag16 F32 N16 O45'
_chemical_formula_weight         4683.93
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   50.0474(6)
_cell_length_b                   50.0474(6)
_cell_length_c                   32.7348(4)
_cell_measurement_reflns_used    60504
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.6610
_cell_measurement_theta_min      2.1040
_cell_volume                     71007.4(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   28.46  205.96   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   73.7540   69.2560 355

  2 omega  -54.64   81.36   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   73.7540   66.7560 272

  3 omega   -8.04   47.96   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   73.7537  -40.7444 112

  4 phi    154.24  195.74   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
 -23.2440   40.0000   73.7540     -     83
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      0.0100666000
_diffrn_orient_matrix_UB_12      -0.0061445000
_diffrn_orient_matrix_UB_13      0.0000559000
_diffrn_orient_matrix_UB_21      0.0107392000
_diffrn_orient_matrix_UB_22      0.0126486000
_diffrn_orient_matrix_UB_23      0.0119735000
_diffrn_orient_matrix_UB_31      -0.0071456000
_diffrn_orient_matrix_UB_32      -0.0083631000
_diffrn_orient_matrix_UB_33      0.0180644000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            115207
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.759
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_description       needle
_exptl_crystal_F_000             40716
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1862
_refine_ls_number_reflns         28859
_refine_ls_number_restraints     747
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0259P)^2^+2358.1863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                25078
_reflns_number_total             28859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rsta20160031supp2.cif
_cod_data_source_block           ilb1903
_cod_original_cell_volume        71007.5(18)
_cod_database_code               1548413
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5011(7) 0.4989(7)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C6-O1C = C5-O1E = C1D-O17 = C1F-O9
 1.45 with sigma of 0.02
 O1J-C11
 1.45 with sigma of 0.02
 C1K-O12
 1.45 with sigma of 0.02
 C0AA-O14
 1.45 with sigma of 0.02
 C1I-O10
 1.45 with sigma of 0.02
 C4AA-O3AA
 1.45 with sigma of 0.02
 C1L-O1B
 1.45 with sigma of 0.02
 O1O-C6AA
 1.45 with sigma of 0.02
 O1M-C1G
 1.45 with sigma of 0.02
 C1N-O15
 1.45 with sigma of 0.02
 C1P-O1H
 1.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O15 \\sim C1N: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
N11 \\sim N21 \\sim N0AA \\sim N18 \\sim N1 \\sim N14 \\sim N16 \\sim N31 \\sim
N33 \\sim N35 \\sim N37 \\sim N44 \\sim N1X \\sim N2P: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.002
C16 \\sim C19 \\sim C25 \\sim C32 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim
C42 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C13 \\sim
C18 \\sim C1A \\sim C1E \\sim C5AA \\sim C3AA \\sim C1J \\sim C8AA \\sim C2AA
\\sim N10 \\sim C21 \\sim C22 \\sim C23 \\sim C7AA \\sim C1O \\sim C26 \\sim
C27 \\sim C28 \\sim C1AA \\sim C30 \\sim C1Q \\sim C1R \\sim C1S \\sim C34
\\sim C1T \\sim C1U \\sim C37 \\sim C1V \\sim C1W \\sim C1Y \\sim C1Z \\sim C44
\\sim C2A \\sim C2C \\sim C2D \\sim C2E \\sim C2G \\sim N2H \\sim C2I \\sim C2J
\\sim C2K \\sim C2M \\sim C2N \\sim C2O \\sim C2Q \\sim C2R \\sim C2S \\sim C2T
\\sim C2U \\sim C2V \\sim C2W \\sim C2X \\sim C2Z \\sim C3A \\sim C3C \\sim C3D
\\sim C3E \\sim C3F \\sim C3H \\sim C3I \\sim C3J \\sim C3K \\sim C3L \\sim C3M
\\sim C3N \\sim C3P \\sim C3Q \\sim C3T \\sim C3U \\sim C3V \\sim C3W \\sim C3X
\\sim C3Z \\sim C4B \\sim C4C \\sim C4D \\sim C1 \\sim C7 \\sim C1C \\sim C8
\\sim C2 \\sim C3 \\sim C4 \\sim O17 \\sim O1C \\sim O9 \\sim O1E \\sim O14
\\sim O10 \\sim C11 \\sim O12 \\sim O15 \\sim O1B \\sim O3AA: within 1.7A with
sigma of 0.002 and sigma for terminal atoms of 0.002
C1R \\sim O22: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C2N \\sim O5AA \\sim O43: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
N33 \\sim C2Q \\sim C2A \\sim C2D \\sim C3J: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
N21 \\sim C38 \\sim C8AA \\sim N1 \\sim C45 \\sim C28: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N31) = Uanis(C2R) = Uanis(C1Z)
5. Rigid body (RIGU) restrains
 F19, F1E, O30, O3, C1E, C1O, F2, O27, F1A, C18, C3AA, O28
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1, C8AA, C3X, C38, C3U, N21, C45, C32, C28, C2E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N31, C2R, C1Z, N37, C2AA, C3I, C46, C3P, C23, C3L
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1U, C2I, N14, C3K, C3E
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O22, C1R, O28, O16, C42, O1A, C5AA, F1K, F1H, C4, F1G, F9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1R, O22, Ag6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N33, C2A, C2D, C2Q, C3J, Ag14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2N, O5AA, O43, Ag15, Ag3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C1N(0.5) O15(0.5) O1O(0.5) C6AA(0.5)
7.a Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C1Q(H1QA,
 H1QB,H1QC), C1S(H1SA,H1SB,H1SC), C1U(H1UA,H1UB,H1UC), C1Z(H1ZA,H1ZB,H1ZC),
 C2D(H2DA,H2DB,H2DC), C2E(H2EA,H2EB,H2EC), C2S(H2SA,H2SB,H2SC), C2T(H2TA,H2TB,
 H2TC), C2W(H2WA,H2WB,H2WC), C2X(H2XA,H2XB,H2XC), C3A(H3AA,H3AB,H3AC), C3E(H3EA,
 H3EB,H3EC), C3F(H3FA,H3FB,H3FC), C3I(H3IA,H3IB,H3IC), C3J(H3JA,H3JB,H3JC),
 C3L(H3LA,H3LB,H3LC), C3M(H3MA,H3MB,H3MC), C3N(H3NA,H3NB,H3NC), C3Q(H3QA,H3QB,
 H3QC), C3U(H3UA,H3UB,H3UC), C3X(H3XA,H3XB,H3XC), C3Z(H3ZA,H3ZB,H3ZC), C4B(H4BA,
 H4BB,H4BC), C4C(H4CA,H4CB,H4CC), C4D(H4DA,H4DB,H4DC)
;
_shelx_res_checksum              25218
_shelx_hkl_checksum              91670
_olex2_submission_special_instructions 'No special instructions were received'