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_1547536
_publ_section_title
;
 Assembly of strongly phosphorescent hetero-bimetallic and -trimetallic
 [2]catenane structures based on a coinage metal alkynyl system
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03529B
_journal_year                    2017
_chemical_formula_moiety         'C192 H252 Au6 Cu6'
_chemical_formula_sum            'C192 H252 Au6 Cu6'
_chemical_formula_weight         4122.96
_chemical_name_systematic        3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-25 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7200(11)
_cell_length_b                   30.9053(14)
_cell_length_c                   52.473(2)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    220
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.44
_cell_volume                     40088(3)
_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      220.02
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            244098
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.140
_diffrn_reflns_theta_max         25.140
_diffrn_reflns_theta_min         2.110
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.038
_exptl_absorpt_correction_T_max  0.2046
_exptl_absorpt_correction_T_min  0.0957
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1177 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.4677.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       Block
_exptl_crystal_F_000             16416
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/acetonitrile'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.093
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         8933
_refine_ls_number_restraints     1323
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1095P)^2^+1012.9807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.2274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5701
_reflns_number_total             8933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03529b2.cif
_cod_data_source_block           mo_chem0005_0m
_cod_database_code               1547536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C33, C41}
{C71, C17}
{C18, C72}
3. Restrained distances
 C51-C37 = C53-C51 = C52-C51 = C54-C51 = C58-C55 = C56-C55 = C57-C55 = C55-C47
 1.53 with sigma of 0.02
 C45-C65 = C66-C65 = C67-C65 = C65-C68
 1.53 with sigma of 0.02
 C9-C10A = C9-C12 = C9-C12A = C9-C11 = C9-C11A = C9-C10
 1.53 with sigma of 0.02
 C5-C13 = C5-C13A = C14-C13 = C16-C13 = C15-C13 = C15A-C13A = C14A-C13A = C16A-
 C13A
 1.53 with sigma of 0.02
 C27-C25 = C28-C25 = C26-C25 = C27A-C25A = C28A-C25A = C26A-C25A
 1.53 with sigma of 0.02
 C77-C25A = C25-C23
 1.53 with sigma of 0.02
 C29-C21 = C75-C29A = C30-C29 = C30A-C29A = C31-C29 = C31A-C29A = C32A-C29A =
 C32-C29
 1.53 with sigma of 0.02
 C61-C39 = C61-C62 = C61-C63
 1.53 with sigma of 0.02
 C64-C61
 1.53 with sigma of 0.02
 C28-C23 = C27-C23 = C26-C23
 2.52 with sigma of 0.04
 C27A-C77 = C26A-C77 = C28A-C77
 2.52 with sigma of 0.04
 C21-C30 = C21-C31 = C21-C32 = C30-C31 = C31-C32 = C32-C30
 2.52 with sigma of 0.04
 C75-C30A = C75-C31A = C75-C32A = C30A-C31A = C31A-C32A = C32A-C30A
 2.52 with sigma of 0.04
 C26-C27 = C27-C28 = C28-C26 = C26A-C27A = C27A-C28A = C28A-C26A
 2.52 with sigma of 0.04
 C54-C52 = C58-C57
 2.52 with sigma of 0.04
 C54-C53 = C56-C57
 2.52 with sigma of 0.04
 C52-C53 = C58-C56
 2.52 with sigma of 0.04
 C58-C47 = C54-C37
 2.52 with sigma of 0.04
 C57-C47 = C52-C37
 2.52 with sigma of 0.04
 C53-C37 = C56-C47
 2.52 with sigma of 0.04
 C63-C39
 2.52 with sigma of 0.04
 C66-C45
 2.52 with sigma of 0.04
 C67-C45
 2.52 with sigma of 0.04
 C68-C45
 2.52 with sigma of 0.04
 C66-C67
 2.52 with sigma of 0.04
 C66-C68
 2.52 with sigma of 0.04
 C67-C68
 2.52 with sigma of 0.04
 C10A-C7
 2.52 with sigma of 0.04
 C12-C7
 2.52 with sigma of 0.04
 C12A-C7
 2.52 with sigma of 0.04
 C11-C7
 2.52 with sigma of 0.04
 C11A-C7
 2.52 with sigma of 0.04
 C10-C7
 2.52 with sigma of 0.04
 C14-C16 = C16A-C14A
 2.52 with sigma of 0.04
 C16-C15 = C14A-C15A
 2.52 with sigma of 0.04
 C15-C14 = C15A-C16A
 2.52 with sigma of 0.04
 C16A-C5
 2.52 with sigma of 0.04
 C15A-C5
 2.52 with sigma of 0.04
 C14A-C5
 2.52 with sigma of 0.04
 C14-C5
 2.52 with sigma of 0.04
 C16-C5
 2.52 with sigma of 0.04
 C15-C5
 2.52 with sigma of 0.04
 C65-C46
 2.52 with sigma of 0.04
 C65-C44
 2.52 with sigma of 0.04
 C63-C62
 2.52 with sigma of 0.04
 C62-C39
 2.52 with sigma of 0.04
 C64-C63
 2.52 with sigma of 0.04
 C64-C62
 2.52 with sigma of 0.04
 C64-C39
 2.52 with sigma of 0.04
4. Restrained planarity
 C34, C35, C36, C37, C38, C39, C40
 with sigma of 0.1
 C42, C43, C44, C45, C46, C65
 with sigma of 0.1
 C19, C20, C21, C22, C23, C24
 with sigma of 0.1
 C73, C74, C75, C76, C77, C78
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C33) = Uanis(C41)
Uanis(C34) = Uanis(C42)
Uanis(C33) = Uanis(C41)
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
Uanis(C71) = Uanis(C17)
Uanis(C18) = Uanis(C72)
6. Same fragment restrains
{C17, C18, C19, C20, C21, C22, C23, C24} sigma for 1-2: 0.02, 1-3: 0.04
{C33, C34, C35, C36, C37, C38, C39, C40} sigma for 1-2: 0.02, 1-3: 0.04
{C71, C72, C73, C74, C75, C76, C77, C78} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1, C2, C3, C4, C5, C6, C7, C8}
7. Others
 Sof(C41)=Sof(C42)=Sof(C43)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(C46)=Sof(H46)=
 Sof(C45)=Sof(C44)=Sof(H44)=Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C65)=Sof(C66)=Sof(H66A)=Sof(H66B)=
 Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=1-FVAR(1)
 Sof(C33)=Sof(C34)=Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(C38)=Sof(H38)=
 Sof(C39)=Sof(C40)=Sof(H40)=Sof(C51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C61)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(2)
 Sof(C13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(3)
 Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(3)
 Sof(C71)=Sof(C72)=Sof(C73)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(C76)=Sof(H76)=
 Sof(C77)=Sof(C78)=Sof(H78)=Sof(C25A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C29A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(4)
 Sof(C17)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(4)
8.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C20(H20), C22(H22), C24(H24), C36(H36), C38(H38),
 C40(H40), C48(H48), C46(H46), C44(H44), C74(H74), C76(H76), C78(H78)
8.b Fitted hexagon refined as free rotating group:
 C43(C48,C47,C46,C45,C44)
8.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C63(H63A,
 H63B,H63C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C12A(H12D,H12E,H12F), C11A(H11D,H11E,
 H11F), C10A(H10D,H10E,H10F), C14A(H14D,H14E,H14F), C16A(H16D,H16E,H16F),
 C15A(H15D,H15E,H15F), C27A(H27D,H27E,H27F), C26A(H26D,H26E,H26F), C28A(H28D,
 H28E,H28F), C32A(H32D,H32E,H32F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'