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_7057946
_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         'C86 H72 Ag12 Cr2 F12 N6 O15 S6'
_chemical_formula_sum            'C86 H72 Ag12 Cr2 F12 N6 O15 S6'
_chemical_formula_weight         3248.29
_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             2017-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                66.079(5)
_cell_angle_beta                 72.957(4)
_cell_angle_gamma                82.717(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5753(3)
_cell_length_b                   16.3742(8)
_cell_length_c                   17.2297(9)
_cell_measurement_reflns_used    2753
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.7890
_cell_measurement_theta_min      3.3960
_cell_volume                     2607.4(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_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  -23.00   25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -150.0000 48

  2 omega  -11.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323 -101.0000   -4.0000 37

  3 omega   45.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   57.0000 -120.0000 44

  4 omega    2.00   41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -37.0000  -30.0000 39

  5 omega  -49.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000   90.0000 82

  6 omega   14.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   37.0000 -150.0000 76

  7 omega   32.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000   60.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0152162000
_diffrn_orient_matrix_UB_12      0.0423642000
_diffrn_orient_matrix_UB_13      -0.0299142000
_diffrn_orient_matrix_UB_21      0.0122078000
_diffrn_orient_matrix_UB_22      -0.0173446000
_diffrn_orient_matrix_UB_23      -0.0331735000
_diffrn_orient_matrix_UB_31      -0.0673883000
_diffrn_orient_matrix_UB_32      -0.0122604000
_diffrn_orient_matrix_UB_33      0.0137111000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17105
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99097
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_description       block
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4711
_reflns_number_total             9217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04965c2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7057946--7057948.cif.'
_cod_database_code               7057946
_chemical_oxdiff_formula         C1H1O1N1S1Cr1F1Ag1
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.652
_reflns_odcompleteness_completeness 86.23
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2B-C37B \\sim F3B-C37B \\sim F1A-C37A \\sim F1B-C37B \\sim F2A-C37A \\sim
F3A-C37A
 with sigma of 0.01
 C37A-C36A \\sim C37B-C36B
 with sigma of 0.01
 F4A-C35 \\sim F6B-C35 \\sim F5A-C35 \\sim F5B-C35 \\sim F6A-C35 \\sim F4B-C35
 with sigma of 0.01
 C18B-C17B \\sim C17B-C16B \\sim C21B-C16B \\sim C21B-C20B \\sim C20B-C19B
\\sim C19B-C18B
 with sigma of 0.01
 C13B-C12 \\sim C13A-C12
 with sigma of 0.01
 C22B-C13B \\sim C14B-C13B \\sim C15B-C14B \\sim C16B-C15B \\sim C21B-C16B
\\sim C22B-C21B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C22A) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C20B) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C19B) \\sim Ueq,
Uanis(C18B) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C17B) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq,
Uanis(C15B) \\sim Ueq, Uanis(C21B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F4A) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F5B)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F4B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C36A) \\sim Ueq, Uanis(C36B) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(F1B)
\\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(F1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C36B)=Sof(C37B)=Sof(F3B)=Sof(F2B)=Sof(F1B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-
 FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C36A)=Sof(C37A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 FVAR(1)
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) C13A(0.5) C13B(0.5)
 C14A(0.5) H14A(0.5) C15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
 C18A(0.5) H18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) C21A(0.5) H21A(0.5)
 C22A(0.5) H22A(0.5) C14B(0.5) H14B(0.5) C15B(0.5) H15B(0.5) C16B(0.5)
 C17B(0.5) H17B(0.5) C18B(0.5) H18B(0.5) C19B(0.5) H19B(0.5) C21B(0.5)
 C20B(0.5) H20B(0.5) C22B(0.5) H22B(0.5) O8(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C12(H12C,H12D), C23(H23A,H23B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C25(H25), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C14A(H14A), C16A(H16A),
 C17A(H17A), C18A(H18A), C19A(H19A), C21A(H21A), C22A(H22A), C14B(H14B),
 C15B(H15B), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B), C22B(H22B)
5.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              85309
_shelx_hkl_checksum              33166
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'