A robust wave-like silver‒thiolate chain based metal‒organic network: synthesis, structure and luminescence
Wang, Jie; Li, Yan-Ling; Wang, Zhao-Yang; Zang, Shuang-Quan; CrystEngComm 21 (2019) 2264–; doi:10.1039/C9CE00054B

data_7232469
_publ_section_title
;
 A robust wave-like silver--thiolate chain based metal--organic network:
 synthesis, structure and luminescence
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2264
_journal_paper_doi               10.1039/C9CE00054B
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C26 H42 Ag5 F3 N1.5 O2 S4'
_chemical_formula_sum            'C26 H42 Ag5 F3 N1.5 O2 S4'
_chemical_formula_weight         1132.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-28
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.02.06 svn.r3384 for OlexSys, GUI svn.r5312)
;
_audit_update_record
;
2019-01-11 deposited with the CCDC.    2019-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7277(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.28107(12)
_cell_length_b                   25.8112(3)
_cell_length_c                   11.74661(12)
_cell_measurement_reflns_used    10857
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3530
_cell_measurement_theta_min      4.2170
_cell_volume                     3632.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.993
_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     52.00  82.00   0.50    0.50    --   45.50 -57.00 -60.00   60
  2  \w     20.00 138.00   0.50    0.50    --  100.10 -61.00 -60.00  236
  3  \w     59.00 162.00   0.50    0.50    --  100.10  45.00-120.00  206
  4  \w     92.00 131.00   0.50    0.50    --   45.50  82.00-180.00   78
  5  \w     11.00 143.00   0.50    0.50    --  100.10 -82.00 -60.00  264
  6  \w     59.00 190.00   0.50    0.50    --  100.10  45.00-150.00  262
  7  \w     94.00 132.00   0.50    0.50    --   45.50  82.00 120.00   76
  8  \w     89.00 132.00   0.50    0.50    --   45.50  82.00-120.00   86
  9  \w     89.00 127.00   0.50    0.50    --   45.50  82.00-150.00   76
 10  \w    -41.00  50.00   0.50    0.50    --   45.50 -57.00 -60.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150217000
_diffrn_orient_matrix_UB_12      -0.0584736000
_diffrn_orient_matrix_UB_13      0.0172675000
_diffrn_orient_matrix_UB_21      0.1201833000
_diffrn_orient_matrix_UB_22      -0.0033340000
_diffrn_orient_matrix_UB_23      0.0736526000
_diffrn_orient_matrix_UB_31      -0.0432544000
_diffrn_orient_matrix_UB_32      0.0112674000
_diffrn_orient_matrix_UB_33      0.1111983000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16453
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.745
_exptl_absorpt_correction_T_max  0.239
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             2202
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.109
_refine_diff_density_max         2.149
_refine_diff_density_min         -2.577
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6429
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0677P)^2^+23.5860P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5923
_reflns_number_total             6429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00054b2.cif
_cod_data_source_block           20161010g4-2
_cod_depositor_comments          'Adding full bibliography for 7232469.cif.'
_cod_original_cell_volume        3632.06(6)
_cod_original_formula_sum        'C26 H42 Ag5 F3 N1.50 O2 S4'
_cod_database_code               7232469
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C26H41Ag5F3N1.5O2S4
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 99.23
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C17
 1.53 with sigma of 0.01
 C16-C14 \\sim C14-C15
 with sigma of 0.01
 C7-C6 \\sim C6-C8
 with sigma of 0.01
 C16A-C14A \\sim C14A-C15A
 with sigma of 0.01
 C16-C13 \\sim C16A-C13 \\sim C14-C13 \\sim C14A-C13 \\sim C15-C13 \\sim
C15A-C13
 with sigma of 0.01
 C8A-C7A \\sim C7A-C6A
 with sigma of 0.01
 C7-C5 \\sim C7A-C5 \\sim C8-C5 \\sim C8A-C5 \\sim C5-C6A \\sim C5-C6 \\sim
S2-C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(Ag4A) \\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(C14A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(S4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=1-FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(1)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(2)
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(2)
 Sof(Ag4A)=1-FVAR(3)
 Sof(Ag4)=FVAR(3)
 Fixed Sof: Ag1(0.4) Ag1A(0.6) N2(0.5) H2A(0.5) H2B(0.5)
5.a Rotating group:
 N2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25)
5.c Idealised Me refined as rotating group:
 C2(H2C,H2D,H2E), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C6A(H6AA,
 H6AB,H6AC), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,
 H8AB,H8AC), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15(H15A,H15B,H15C), C15A(H15D,H15E,
 H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.794