Investigating the influence of a CrO42−/Cr2O72− template in the formation of a series of silver‒chalcogenide clusters
Li, Yan-Ling; Xu, Qing-Qing; Li, Si; Huang, Ren-Wu; Liu, Xiao-Fei; Wei, Yong-Li; Zang, Shuang-Quan; New Journal of Chemistry 43 (2019) 115–; doi:10.1039/C8NJ04965C

data_7057948
_publ_section_title
;
 Investigating the influence of a CrO42&#x2212;/Cr2O72&#x2212; template in
 the formation of a series of silver--chalcogenide clusters
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              115
_journal_paper_doi               10.1039/C8NJ04965C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C106 H108 Ag14 F24 N6 O22 S6'
_chemical_formula_sum            'C106 H108 Ag14 F24 N6 O22 S6'
_chemical_formula_weight         3976.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.109(13)
_cell_length_b                   26.729(9)
_cell_length_c                   29.365(13)
_cell_measurement_reflns_used    6879
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.1460
_cell_measurement_theta_min      3.0670
_cell_volume                     13429(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -15.00   18.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   90.0000 66

  2 omega   23.00   54.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   19.0000   60.0000 62

  3 omega   -4.00   82.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   19.0000 -150.0000 172
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0328726000
_diffrn_orient_matrix_UB_12      -0.0042993000
_diffrn_orient_matrix_UB_13      -0.0145504000
_diffrn_orient_matrix_UB_21      0.0214981000
_diffrn_orient_matrix_UB_22      -0.0096064000
_diffrn_orient_matrix_UB_23      0.0188104000
_diffrn_orient_matrix_UB_31      -0.0145822000
_diffrn_orient_matrix_UB_32      -0.0238971000
_diffrn_orient_matrix_UB_33      -0.0049442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32173
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         11813
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0761P)^2^+27.9625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7614
_reflns_number_total             11813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04965c2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7057946--7057948.cif.'
_cod_original_cell_volume        13429(12)
_cod_database_code               7057948
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1O1S1Ag1
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.670
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C43
 1.32 with sigma of 0.01
 C42-C43
 1.53 with sigma of 0.01
 N1-C45
 1.46 with sigma of 0.01
 C2-C3 = C3-C4 = C4-C9 = C9-C10 = C10-C11 = C11-C2
 1.38 with sigma of 0.01
 C4-C5 = C5-C6 = C6-C7 = C7-C8 = C8-C9 = C9-C4
 1.38 with sigma of 0.01
 C40-C41
 1.55 with sigma of 0.01
 C18-C20 = C20-C22 = C13-C15
 2.35 with sigma of 0.01
 C15-C16 = C16-C17 = C17-C18 = C18-C19 = C19-C20 = C20-C15
 1.38 with sigma of 0.01
 C13-C14 = C14-C15 = C15-C20 = C20-C21 = C21-C22 = C22-C13
 1.38 with sigma of 0.01
 C41-F7 \\sim C41-F8 \\sim C41-F9
 with sigma of 0.01
3. Rigid bond restraints
 F2, C35, C7, C8, C4, C9, F1, C35, F9, C41, C40, C41, C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ag1, S1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 Ag5, S3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 Ag4, S1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 C17, C18, C28, C29, C15, C20, C4, C5, C14, C15, C18, C19, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, C41, C29, C30, F10, C37, C20, C21, C10, C11, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9, C43, C9, C10, C42, C43, N1, C45, C5, C6, C21, C22, C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C36, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, C38, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F8) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F10) \\sim
Ueq, Uanis(F11) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(F7) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33)
5.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_olex2_submission_special_instructions 'No special instructions were received'