Self-assembly of thiolate-protected silver coordination polymers regulated by POMs.
Li, Ya-Hui; Wang, Zhao-Yang; Ma, Bing; Xu, Hong; Zang, Shuang-Quan; Mak, Thomas C. W.; Nanoscale 12 (2020) 10944–10948; doi:10.1039/d0nr00342e

data_1557976
_publ_section_title
;
 Self-assembly of thiolate-protected silver coordination polymers
 regulated by POMs.
;
_journal_issue                   20
_journal_name_full               Nanoscale
_journal_page_first              10944
_journal_page_last               10948
_journal_paper_doi               10.1039/d0nr00342e
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'0.5(C116 H246 Ag36 N10 S24), 3(Mo6 O19), 2(C2 H3 N)'
_chemical_formula_sum            'C62 H129 Ag18 Mo18 N7 O57 S12'
_chemical_formula_weight         5938.01
_chemical_name_systematic        Ag18-Mo6
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-30 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.3167(2)
_cell_length_b                   19.80926(14)
_cell_length_c                   27.71777(16)
_cell_measurement_reflns_used    34004
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.4500
_cell_measurement_theta_min      2.7280
_cell_volume                     14998.74(18)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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     60.00  99.00   0.50    0.70    --   45.50  57.00 -60.00   78
  2  \w     24.00  55.00   0.50    0.70    --   45.50  57.00 -60.00   62
  3  \w     17.00  65.00   0.50    0.70    --   45.50  57.00   0.00   96
  4  \w      7.00 134.00   0.50    0.70    --   45.50  82.00-180.00  254
  5  \w     90.00 127.00   0.50    2.00    --  100.10 -61.00  30.00   74
  6  \w     46.00  86.00   0.50    2.00    --  100.10 -82.00   0.00   80
  7  \w     14.00 122.00   0.50    2.00    --  100.10 -77.00  30.00  216
  8  \w     69.00 102.00   0.50    2.00    --  100.10  45.00 -60.00   66
  9  \w     23.00  49.00   0.50    2.00    --  100.10 -61.00  30.00   52
 10  \w    122.00 172.00   0.50    2.00    --  100.10  45.00 -60.00  100
 11  \w    116.00 146.00   0.50    2.00    --  100.10 -30.00 150.00   60
 12  \w     19.00  92.00   0.50    2.00    --  100.10 -30.00 150.00  146
;
_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      0.0201925000
_diffrn_orient_matrix_UB_12      -0.0322257000
_diffrn_orient_matrix_UB_13      0.0465087000
_diffrn_orient_matrix_UB_21      0.0029035000
_diffrn_orient_matrix_UB_22      -0.0688705000
_diffrn_orient_matrix_UB_23      -0.0256217000
_diffrn_orient_matrix_UB_31      0.0525864000
_diffrn_orient_matrix_UB_32      0.0162197000
_diffrn_orient_matrix_UB_33      -0.0164468000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            56711
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.593
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16598
_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            yellowish
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    2.630
_exptl_crystal_description       block
_exptl_crystal_F_000             11200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.401
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         14604
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0397P)^2^+242.7789P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13574
_reflns_number_total             14604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr00342e2.cif
_cod_data_source_block           ag18-mo6
_cod_depositor_comments
'Adding full bibliography for 1557975--1557976.cif.'
_cod_original_cell_volume        14998.72(18)
_cod_database_code               1557976
_shelxl_version_number           2013-2
_chemical_oxdiff_usercomment     'C H O N '
_shelx_estimated_absorpt_t_max   0.140
_shelx_estimated_absorpt_t_min   0.140
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C29 = C30-C29 = C29-C31
 1.53 with sigma of 0.01
 C27-C25 = C28-C25 = C26-C25
 1.53 with sigma of 0.01
 C21-C22 = C21-C24 = C23-C21
 1.53 with sigma of 0.01
 C18-C17 = C17-C19 = C17-C20
 1.53 with sigma of 0.01
 C2A-C1A = C2B-C1B
 1.53 with sigma of 0.01
 N4B-C1B = N4A-C1A
 1.1 with sigma of 0.01
 C8-C7
 1.5 with sigma of 0.02
 C30-C29 = C32-C29 = C29-C31
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Ag2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Ag9A)=1-FVAR(1)
 Sof(Ag9B)=FVAR(1)
 Fixed Sof: N4A(0.5) C1A(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) N4B(0.5)
 C1B(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5) N2(0.5) C7(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5)
5.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C8(H8A,H8B,H8C), C4(H4A,
 H4B,H4C)
;
_shelx_res_checksum              38928
_shelx_fab_checksum              25001
_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 3.887
_oxdiff_exptl_absorpt_empirical_full_min 0.600