Assembly of strongly phosphorescent hetero-bimetallic and -trimetallic [2]catenane structures based on a coinage metal alkynyl system
Chang, Xiao-Yong; Xu, Guang-Tao; Cao, Bei; Wang, Juan-Yu; Huang, Jie-Sheng; Che, Chi-Ming; Chem. Sci.  (2017) –; doi:10.1039/C7SC03529B

data_1547537
_publ_section_title
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 Assembly of strongly phosphorescent hetero-bimetallic and -trimetallic
 [2]catenane structures based on a coinage metal alkynyl system
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_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03529B
_journal_year                    2017
_chemical_formula_moiety         'C72 H108 Ag1.81 Au10.19'
_chemical_formula_sum            'C72 H108 Ag1.8 Au10.2'
_chemical_formula_weight         3176.36
_chemical_name_systematic        tBuAuAg51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-06-05 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.086(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.818(3)
_cell_length_b                   12.9632(13)
_cell_length_c                   25.496(3)
_cell_measurement_temperature    296(2)
_cell_volume                     8480.0(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72045
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.609
_diffrn_reflns_theta_max         67.609
_diffrn_reflns_theta_min         3.445
_exptl_absorpt_coefficient_mu    35.733
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_F_000             5721
_exptl_crystal_preparation       ', Luminescent'
_refine_diff_density_max         7.055
_refine_diff_density_min         -2.871
_refine_diff_density_rms         0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          1.305
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1688P)^2^+324.0992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2404
_refine_ls_wR_factor_ref         0.2438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7038
_reflns_number_total             7478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03529b2.cif
_cod_data_source_block           cxy515_0m
_cod_original_cell_volume        8480.1(15)
_cod_original_formula_sum        'C72 H108 Ag1.80 Au10.20'
_cod_database_code               1547537
_olex2_refinement_description
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1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C00N = C4AA-C13A = C4AA-C19A = C19-C00N = C4AA-C14A = C14-C00N
 1.53 with sigma of 0.02
 C17-C00J = C5AA-C17A = C16-C00J = C5AA-C16A = C6AA-C5AA = C00M-C00J
 1.53 with sigma of 0.02
 C20A-C15A = C20-C15 = C3AA-C15 = C3AB-C15A = C27-C15 = C27A-C15A
 1.53 with sigma of 0.02
 C8AA-C48A = C8AA-C2AB = C48-C00H = C8AA-C24A = C24-C00H = C2AA-C00H
 1.53 with sigma of 0.02
 C11A-C00P = C26A-C00P = C7AB-C00P = C11-C00O = C7AA-C00O = C26-C00O
 1.53 with sigma of 0.02
 C13-C19 = C19A-C13A
 2.52 with sigma of 0.04
 C19-C14 = C14A-C19A
 2.52 with sigma of 0.04
 C14A-C13A = C14-C13
 2.52 with sigma of 0.04
 C17-C16 = C17A-C16A
 2.52 with sigma of 0.04
 C17A-C6AA = C00M-C17
 2.52 with sigma of 0.04
 C00M-C16 = C6AA-C16A
 2.52 with sigma of 0.04
 C3AB-C20A = C3AA-C20
 2.52 with sigma of 0.04
 C3AB-C27A = C3AA-C27
 2.52 with sigma of 0.04
 C20-C27 = C20A-C27A
 2.52 with sigma of 0.04
 C48A-C2AB = C2AA-C24
 2.52 with sigma of 0.04
 C48-C24 = C24A-C48A
 2.52 with sigma of 0.04
 C48-C2AA = C2AB-C24A
 2.52 with sigma of 0.04
 C11-C7AA = C7AB-C11A
 2.52 with sigma of 0.04
 C11A-C26A = C11-C26
 2.52 with sigma of 0.04
 C7AB-C26A = C7AA-C26
 2.52 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C13A \\sim C4AA \\sim C19A \\sim C14A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C26A \\sim C00P \\sim C11A \\sim C7AB: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C16A \\sim C5AA \\sim C17A \\sim C6AA: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C48 \\sim C00H \\sim C24 \\sim C2AA: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C00B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00N) = Uanis(C4AA)
Uanis(C19) = Uanis(C19A)
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
Uanis(C00J) = Uanis(C5AA)
Uanis(C17) = Uanis(C17A)
Uanis(C16) = Uanis(C16A)
Uanis(C00M) = Uanis(C6AA)
Uanis(C15) = Uanis(C15A)
Uanis(C3AA) = Uanis(C3AB)
Uanis(C27) = Uanis(C27A)
Uanis(C20) = Uanis(C20A)
Uanis(C00H) = Uanis(C8AA)
Uanis(C2AA) = Uanis(C2AB)
Uanis(C48) = Uanis(C48A)
Uanis(C24) = Uanis(C24A)
Uanis(C00O) = Uanis(C00P)
Uanis(C11) = Uanis(C11A)
Uanis(C7AA) = Uanis(C7AB)
Uanis(C26) = Uanis(C26A)
Uanis(Ag06) = Uanis(Au)
Uanis(Au05) = Uanis(Ag1)
4. Others
 Sof(Au)=1-FVAR(1)
 Sof(Ag06)=FVAR(1)
 Sof(C4AA)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(2)
 Sof(C00N)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
 Sof(C5AA)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(3)
 Sof(C00J)=Sof(C00M)=Sof(H00A)=Sof(H00B)=Sof(H00C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
 Sof(C15A)=Sof(C3AB)=Sof(H3AD)=Sof(H3AE)=Sof(H3AF)=Sof(C27A)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(4)
 Sof(C15)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(4)
 Sof(C8AA)=Sof(C2AB)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=Sof(C48A)=Sof(H48D)=
 Sof(H48E)=Sof(H48F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(5)
 Sof(C00H)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(5)
 Sof(C00P)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C7AB)=Sof(H7AD)=
 Sof(H7AE)=Sof(H7AF)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(6)
 Sof(C00O)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C7AA)=Sof(H7AA)=
 Sof(H7AB)=Sof(H7AC)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(6)
 Sof(Ag1)=1-FVAR(7)
 Sof(Au05)=FVAR(7)
5.a Idealised Me refined as rotating group:
 C00M(H00A,H00B,H00C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C),
 C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C0AA(H0AA,H0AB,H0AC), C17(H17A,
 H17B,H17C), C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C3AA(H3AA,H3AB,H3AC),
 C27(H27A,H27B,H27C), C19A(H19D,H19E,H19F), C14A(H14D,H14E,H14F), C13A(H13D,
 H13E,H13F), C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F), C6AA(H6AA,H6AB,H6AC),
 C11(H11A,H11B,H11C), C7AA(H7AA,H7AB,H7AC), C26(H26A,H26B,H26C), C3AB(H3AD,H3AE,
 H3AF), C27A(H27D,H27E,H27F), C20A(H20D,H20E,H20F), C2AB(H2AD,H2AE,H2AF),
 C48A(H48D,H48E,H48F), C24A(H24D,H24E,H24F), C11A(H11D,H11E,H11F), C7AB(H7AD,
 H7AE,H7AF), C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              61240
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'