Porphyrinic Silver Cluster Assembled Material for Simultaneous Capture and Photocatalysis of Mustard-Gas Simulant.
Cao, Man; Pang, Rui; Wang, Qian-You; Han, Zhen; Wang, Zhao-Yang; Dong, Xi-Yan; Li, Shun-Fang; Zang, Shuang-Quan; Mak, Thomas C. W.; Journal of the American Chemical Society 141 (2019) 14505–14509; doi:10.1021/jacs.9b05952

data_4127624
_publ_section_title
;
 Porphyrinic Silver Cluster Assembled Material for Simultaneous Capture
 and Photocatalysis of Mustard-Gas Simulant.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14505
_journal_page_last               14509
_journal_paper_doi               10.1021/jacs.9b05952
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C76 H80 Ag12 F18 N8 O12 S6'
_chemical_formula_sum            'C76 H80 Ag12 F18 N8 O12 S6'
_chemical_formula_weight         3126.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                61.4520(10)
_cell_angle_beta                 68.2290(10)
_cell_angle_gamma                67.3880(10)
_cell_formula_units_Z            1
_cell_length_a                   14.77100(10)
_cell_length_b                   15.4918(2)
_cell_length_c                   15.6410(2)
_cell_measurement_reflns_used    49937
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.9640
_cell_measurement_theta_min      3.3110
_cell_volume                     2823.93(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -37.00  67.00   0.50    0.50    --    0.00  82.00 -30.00  208
  2  \w    -30.00  29.00   0.50    0.50    --    0.00 -38.00 150.00  118
  3  \w    -35.00  12.00   0.50    0.50    --    0.00  77.00-120.00   94
  4  \w    -20.00  21.00   0.50    0.50    --    0.00 -57.00 150.00   82
  5  \w     48.00  88.00   0.50    0.50    --    0.00  19.00   0.00   80
  6  \w    -87.00 -39.00   0.50    0.50    --    0.00 -57.00 150.00   96
  7  \w    -70.00 -39.00   0.50    0.50    --    0.00 -38.00 150.00   62
  8  \w     -5.00  43.00   0.50    0.50    --    0.00  19.00   0.00   96
  9  \w    -29.00  89.00   0.50    0.50    --    0.00  38.00  90.00  236
 10  \w    -29.00  72.00   0.50    0.50    --    0.00  57.00-120.00  202
 11  \w     26.00  52.00   0.50    0.50    --    0.00  77.00-120.00   52
 12  \w    -45.00  -9.00   0.50    0.50    --    0.00  19.00   0.00   72
 13  \w    136.00 179.00   0.50    0.50    --   97.60  81.00   9.21   86
 14  \w     60.00  86.00   0.50    0.50    --   97.60  81.00   9.21   52
 15  \w     60.00  93.00   0.50    0.50    --   97.60  82.00-112.46   66
 16  \w     60.00  89.00   0.50    0.50    --   97.60  80.00  85.06   58
 17  \w    149.00 182.00   0.50    0.50    --   97.60  80.00 101.30   66
 18  \w    160.00 186.00   0.50    0.50    --   97.60  78.00-160.53   52
 19  \w     63.00 187.00   0.50    0.50    --   97.60  75.00  48.97  248
 20  \w    108.00 187.00   0.50    0.50    --   97.60  82.00 -30.00  158
 21  \w     62.00  88.00   0.50    0.50    --   97.60  82.00 -30.00   52
 22  \w     60.00  85.00   0.50    0.50    --   97.60  80.00 101.30   50
 23  \w     62.00 120.00   0.50    0.50    --   97.60  77.00  60.00  116
 24  \w     62.00  88.00   0.50    0.50    --   97.60  77.00 -30.00   52
 25  \w     67.00  93.00   0.50    0.50    --   97.60  61.00  60.00   52
 26  \w     62.00  88.00   0.50    0.50    --   97.60  77.00  30.00   52
 27  \w     60.00  87.00   0.50    0.50    --   97.60  82.00 120.00   54
 28  \w     62.00 172.00   0.50    0.50    --   97.60  77.00-120.00  220
 29  \w     62.00  87.00   0.50    0.50    --   97.60  77.00 -60.00   50
 30  \w     60.00  86.00   0.50    0.50    --   97.60  82.00 -90.00   52
 31  \w     28.00 134.00   0.50    0.50    --   97.60 -82.00  30.00  212
 32  \w     62.00  87.00   0.50    0.50    --   97.60  77.00 -90.00   50
 33  \w    153.00 179.00   0.50    0.50    --   97.60  80.00 144.98   52
 34  \w     61.00  87.00   0.50    0.50    --   97.60  78.00-160.53   52
 35  \w     69.00 131.00   0.50    0.50    --   97.60  45.00 -60.00  124
 36  \w     60.00  85.00   0.50    0.50    --   97.60  82.00 -60.00   50
 37  \w     69.00 184.00   0.50    0.50    --   97.60  45.00-180.00  230
 38  \w     61.00 132.00   0.50    0.50    --   97.60 -82.00 -90.00  142
 39  \w      8.00 135.00   0.50    0.50    --   97.60 -82.00 -30.00  254
 40  \w     60.00  86.00   0.50    0.50    --   97.60  80.00 144.98   52
 41  \w     61.00  86.00   0.50    0.50    --   97.60  79.00 117.48   50
 42  \w     60.00  86.00   0.50    0.50    --   97.60  82.00-120.00   52
 43  \w     69.00  96.00   0.50    0.50    --   97.60  45.00  30.00   54
 44  \w    110.00 182.00   0.50    0.50    --   97.60  45.00  30.00  144
 45  \w     69.00 178.00   0.50    0.50    --   97.60  51.00 150.62  218
 46  \w     67.00 155.00   0.50    0.50    --   97.60  61.00 120.00  176
 47  \w     62.00  88.00   0.50    0.50    --   97.60  77.00-150.00   52
 48  \w     10.00 131.00   0.50    0.50    --   97.60 -82.00-180.00  242
 49  \w     67.00  92.00   0.50    0.50    --   97.60  61.00  30.00   50
 50  \w    120.00 179.00   0.50    0.50    --   97.60  82.00 -90.00  118
 51  \w     65.00  90.00   0.50    0.50    --   97.60  68.00  11.00   50
 52  \w     67.00  93.00   0.50    0.50    --   97.60  61.00-120.00   52
 53  \w     98.00 141.00   0.50    0.50    --   97.60  61.00-120.00   86
 54  \w     67.00  93.00   0.50    0.50    --   97.60  61.00   0.00   52
 55  \w    137.00 177.00   0.50    0.50    --   97.60  82.00-180.00   80
 56  \w     61.00  86.00   0.50    0.50    --   97.60  78.00-130.64   50
 57  \w    107.00 187.00   0.50    0.50    --   97.60  82.00-112.46  160
 58  \w     65.00 182.00   0.50    0.50    --   97.60  66.00-171.69  234
 59  \w     69.00 133.00   0.50    0.50    --   97.60  45.00 120.00  128
 60  \w     60.00  86.00   0.50    0.50    --   97.60  82.00  60.00   52
 61  \w     69.00 173.00   0.50    0.50    --   97.60  50.00 -40.76  208
 62  \w     69.00 176.00   0.50    0.50    --   97.60  45.00  60.00  214
 63  \w     66.00 134.00   0.50    0.50    --   97.60 -82.00 120.00  136
 64  \w     69.00 114.00   0.50    0.50    --   97.60  48.00  -5.85   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0640669000
_diffrn_orient_matrix_UB_12      0.0749661000
_diffrn_orient_matrix_UB_13      0.0513932000
_diffrn_orient_matrix_UB_21      0.0671640000
_diffrn_orient_matrix_UB_22      0.0736446000
_diffrn_orient_matrix_UB_23      -0.0728288000
_diffrn_orient_matrix_UB_31      -0.0697673000
_diffrn_orient_matrix_UB_32      0.0515449000
_diffrn_orient_matrix_UB_33      -0.0730395000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            61810
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.498
_diffrn_reflns_theta_max         66.498
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.028
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9894
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0587P)^2^+12.3367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9589
_reflns_number_total             9894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05952_si_002.cif
_cod_data_source_block           20190222a6-hy
_cod_original_cell_volume        2823.93(7)
_cod_database_code               4127624
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.266
_shelx_estimated_absorpt_t_min   0.074
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F6B-C16B \\sim F5B-C16B \\sim F4B-C16B \\sim F6A-C16A \\sim F4A-C16A \\sim
F5A-C16A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F4A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5B) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(F6B)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F4A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F4A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F6A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F5A(0.5) F5B(0.5) F4A(0.5) F4B(0.5) F6A(0.5) F6B(0.5) C16A(0.5)
 C16B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C27(H27), C26(H26), C37(H37), C33(H33), C20(H20), C19(H19), C22(H22),
 C23(H23), C36(H36), C34(H34), C31(H31), C32(H32)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C), C6(H6A,
 H6B,H6C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C3(H3A,H3B,H3C), C12(H12A,
 H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23868
_shelx_hkl_checksum              61750
_shelx_fab_checksum              21302
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.220
_oxdiff_exptl_absorpt_empirical_full_min 0.561