[Au7Ag9(dppf)3(CF3CO2)7BF4]n: A Linear Nanocluster Polymer from Molecular Au7Ag8 Clusters Covalently Linking by Silver Atoms
Wen, Zhao-Rui; Guan, Zong-Jie; Zhang, Ying; Lin, Yu-Mei; Wang, Quan-Ming; Chemical Communications  (2019) –; doi:10.1039/C9CC05924E

data_7124275
_publ_section_title
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 [Au7Ag9(dppf)3(CF3CO2)7BF4]n: A Linear Nanocluster Polymer from Molecular
 Au7Ag8 Clusters Covalently Linking by Silver Atoms
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05924E
_journal_year                    2019
_chemical_formula_moiety         'C116 H84 Ag9 Au7 F21 Fe3 O14 P6, B F4'
_chemical_formula_sum            'C116 H84 Ag9 Au7 B F25 Fe3 O14 P6'
_chemical_formula_weight         4890.60
_chemical_name_systematic        '[Au7Ag9]n'
_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     dual
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-29 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                88.524(2)
_cell_angle_beta                 86.188(2)
_cell_angle_gamma                65.006(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7746(3)
_cell_length_b                   17.3633(4)
_cell_length_c                   30.4935(6)
_cell_measurement_reflns_used    23957
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.3100
_cell_measurement_theta_min      3.5340
_cell_volume                     7074.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     -6.00  20.25   0.75   13.34    --   -9.18 -99.00  30.00   35
  2  \w    -55.00  35.00   0.75   13.34    --    9.57 -37.00-120.00  120
  3  \w    -16.00  82.25   0.75   13.34    --    9.57  37.00  60.00  131
  4  \w    -20.00  74.50   0.75   13.34    --    9.57  67.00-176.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45544
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.404
_exptl_absorpt_coefficient_mu    8.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_description       block
_exptl_crystal_F_000             4532
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.861
_refine_diff_density_min         -6.108
_refine_diff_density_rms         0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         24649
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1638
_refine_ls_R_factor_gt           0.1468
_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^)+(0.1083P)^2^+1390.3540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3585
_refine_ls_wR_factor_ref         0.3668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19089
_reflns_number_total             24649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05924e2.cif
_cod_data_source_block           207c1-3
_cod_database_code               7124275
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.470
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B49-F32
 1.412 with sigma of 0.02
 B49-F58
 1.412 with sigma of 0.02
 B49-F55
 1.412 with sigma of 0.02
 B49-F200
 1.412 with sigma of 0.02
 F32-F58
 2.301 with sigma of 0.02
 F32-F55
 2.301 with sigma of 0.02
 F32-F200
 2.301 with sigma of 0.02
 F58-F55
 2.301 with sigma of 0.02
 F58-F200
 2.301 with sigma of 0.02
 F200-F55
 2.301 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7DA) = Uanis(C6DA) = Uanis(C9BA) = Uanis(C40) = Uanis(C74) = Uanis(C52)
Uanis(C8AA) = Uanis(C7AA) = Uanis(C96) = Uanis(C42) = Uanis(C62) = Uanis(C64)
Uanis(C45) = Uanis(C23) = Uanis(C41) = Uanis(C6AA) = Uanis(C4EA)
Uanis(C85) = Uanis(C65) = Uanis(C16) = Uanis(C90) = Uanis(C71)
Uanis(C39) = Uanis(C3CA) = Uanis(C4CA) = Uanis(C5CA) = Uanis(C1BA) = Uanis(C84)
Uanis(C80) = Uanis(C28) = Uanis(C3DA) = Uanis(C2DA) = Uanis(C1DA) = Uanis(C73)
Uanis(C3EA) = Uanis(C6CA) = Uanis(C78) = Uanis(C7CA) = Uanis(C8CA) = Uanis(C37)
Uanis(C33) = Uanis(C60) = Uanis(C92) = Uanis(C38) = Uanis(C36)
Uanis(C76) = Uanis(C3BA) = Uanis(C48) = Uanis(C4BA) = Uanis(C88)
Uanis(C75) = Uanis(C3AA) = Uanis(C87) = Uanis(C2AA) = Uanis(C4AA) = Uanis(C54)
Uanis(C5DA) = Uanis(C49) = Uanis(C51) = Uanis(C99) = Uanis(C69) = Uanis(C95)
Uanis(C1EA) = Uanis(C47) = Uanis(C1AA) = Uanis(C53) = Uanis(C13) = Uanis(C46)
Uanis(C72) = Uanis(C98) = Uanis(C30) = Uanis(C32) = Uanis(C18) = Uanis(C91)
Uanis(C56) = Uanis(C7BA) = Uanis(C19) = Uanis(C0AA) = Uanis(C6BA)
Uanis(C67) = Uanis(C5BA) = Uanis(C61) = Uanis(C63) = Uanis(C86)
Uanis(C8DA) = Uanis(C6EA) = Uanis(C2CA) = Uanis(C50) = Uanis(C0CA) = Uanis(C1CA)
Uanis(C0EA) = Uanis(C9DA) = Uanis(C8BA) = Uanis(C57) = Uanis(C66) = Uanis(C29)
Uanis(O1AA) = Uanis(O12) = Uanis(C2EA) = Uanis(O31) = Uanis(C0BA) = Uanis(F35)
= Uanis(F5) = Uanis(F13)
Uanis(O9) = Uanis(C70) = Uanis(O40) = Uanis(C7EA) = Uanis(F36) = Uanis(F83) =
Uanis(F94)
Uanis(C5EA) = Uanis(C2BA) = Uanis(O21) = Uanis(O38)
Uanis(F16) = Uanis(F15) = Uanis(F0AA) = Uanis(C4DA) = Uanis(C43)
Uanis(C81) = Uanis(C5AA) = Uanis(F20) = Uanis(F1AA) = Uanis(F3)
Uanis(C24) = Uanis(O16) = Uanis(O15) = Uanis(C9AA) = Uanis(F87) = Uanis(F43) =
Uanis(F46)
Uanis(Ag0F) = Uanis(C77) = Uanis(C44) = Uanis(F25) = Uanis(F34) = Uanis(F53)
Uiso(F200) = Uiso(B49) = Uiso(F55) = Uiso(F58) = Uiso(F32)
Uanis(C9CA) = Uanis(C8EA) = Uanis(C0DA) = Uanis(C20) = Uanis(C31) = Uanis(C34)
4. Others
 Fixed Sof: O1AA(0.5) O12(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C48(H48), C38(H38), C18(H18), C19(H19), C23(H23), C30(H30),
 C32(H32), C40(H40), C41(H41), C42(H42), C46(H46), C0AA(H0AA), C56(H56),
 C60(H60), C62(H62), C63(H63), C65(H65), C72(H72), C76(H76), C85(H85), C86(H86),
  C90(H90), C92(H92), C98(H98), C99(H99), C29(H29), C4AA(H4AA), C1AA(H1AA),
 C39(H39), C1CA(H1CA), C1BA(H1BA), C8AA(H8AA), C2AA(H2AA), C47(H47), C5BA(H5BA),
  C51(H51), C52(H52), C53(H53), C54(H54), C4BA(H4BA), C61(H61), C6BA(H6BA),
 C3AA(H3AA), C66(H66), C3BA(H3BA), C6AA(H6AA), C0CA(H0CA), C7AA(H7AA), C80(H80),
  C4EA(H4EA), C8BA(H8BA), C2CA(H2CA), C9BA(H9BA), C95(H95), C96(H96),
 C2DA(H2DA), C28(H28), C5CA(H5CA), C37(H37), C4CA(H4CA), C3CA(H3CA), C7DA(H7DA),
  C8CA(H8CA), C1EA(H1EA), C49(H49), C3DA(H3DA), C5DA(H5DA), C9DA(H9DA),
 C6DA(H6DA), C8DA(H8DA), C7CA(H7CA), C75(H75), C6CA(H6CA), C0EA(H0EA),
 C1DA(H1DA), C6EA(H6EA), C3EA(H3EA), C34(H34), C31(H31), C0DA(H0DA), C8EA(H8EA),
  C9CA(H9CA)
5.c Fitted hexagon refined as free rotating group:
 C34(C31,C20,C0DA,C8EA,C9CA)
;
_shelx_res_checksum              53109
_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
;
_platon_squeeze_void_probe_radius 1.20