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_7057947
_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         'C230 H198 Ag30 Cr2 F24 N4 O28 S18'
_chemical_formula_sum            'C230 H198 Ag30 Cr2 F24 N4 O28 S18'
_chemical_formula_weight         7839.09
_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     direct
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
+manual edit
;
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                62.618(2)
_cell_angle_beta                 83.842(2)
_cell_angle_gamma                65.100(2)
_cell_formula_units_Z            1
_cell_length_a                   17.8479(4)
_cell_length_b                   21.0072(4)
_cell_length_c                   21.9628(4)
_cell_measurement_reflns_used    20693
_cell_measurement_temperature    102.3(3)
_cell_measurement_theta_max      28.9260
_cell_measurement_theta_min      3.5220
_cell_volume                     6594.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102.3(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -23.00   23.40   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755  -99.0000  -90.0000 58

  2 omega  -49.00  -18.60   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -77.0000   90.0000 38

  3 omega   -5.00   28.60   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -57.0000 -120.0000 42

  4 omega   19.80   47.00   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -19.0000   90.0000 34

  5 omega  -49.00   33.40   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -57.0000  -30.0000 103

  6 omega  -49.00  -21.80   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -57.0000 -120.0000 34

  7 omega   18.00   45.20   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -77.0000   90.0000 34

  8 omega  -43.00   -3.80   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -19.0000   90.0000 49

  9 omega   -9.00   84.60   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   77.0000 -150.0000 117

 10 omega  -13.00   56.60   0.8000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -99.0000   90.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0267072000
_diffrn_orient_matrix_UB_12      -0.0190030000
_diffrn_orient_matrix_UB_13      0.0058264000
_diffrn_orient_matrix_UB_21      -0.0292959000
_diffrn_orient_matrix_UB_22      0.0266938000
_diffrn_orient_matrix_UB_23      0.0113199000
_diffrn_orient_matrix_UB_31      -0.0192482000
_diffrn_orient_matrix_UB_32      0.0261489000
_diffrn_orient_matrix_UB_33      -0.0342946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61028
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.426
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_description       prism
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.2100
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         1.743
_refine_diff_density_min         -2.461
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1519
_refine_ls_number_reflns         25823
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_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^+10.8827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19347
_reflns_number_total             25823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04965c2.cif
_cod_data_source_block           ag30_sq
_cod_depositor_comments
'Adding full bibliography for 7057946--7057948.cif.'
_cod_database_code               7057947
_chemical_oxdiff_formula         C1H1O1N1S1Ag1
_reflns_odcompleteness_completeness 99.76
_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
 N2-C110 \\sim N2-C104 \\sim N2-C115
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C109) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C115) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C19(H19A,H19B), C21(H21A,H21B), C30(H30A,H30B),
 C36(H36A,H36B), C45(H45A,H45B), C56(H56A,H56B), C58(H58A,H58B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C15(H15),
 C17(H17), C18(H18), C22(H22), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C48(H48), C49(H49),
 C52(H52), C53(H53), C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C65(H65),
  C66(H66), C67(H67), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76),
 C78(H78), C79(H79), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
  C88(H88), C89(H89), C90(H90), C91(H91), C94(H94), C95(H95), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100), C103(H103), C105(H105), C107(H107),
 C108(H108), C109(H109), C112(H112)
4.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C92(H92A,H92B,H92C), C106(H10A,H10B,H10C), C110(H11A,
 H11B,H11C), C114(H11D,H11E,H11F), C115(H11G,H11H,H11I)
;
_shelx_res_checksum              90486
_shelx_hkl_checksum              49602
_shelx_fab_checksum              42467
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'