Defined tetranuclear coinage metal chains
Kaub, Christoph; Lebedkin, Sergei; Bestgen, Sebastian; Köppe, Ralf; Kappes, Manfred M.; Roesky, Peter W.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04705C

data_7120554
_publ_section_title
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 Defined tetranuclear coinage metal chains
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04705C
_journal_year                    2017
_chemical_formula_moiety         'C58 H48 Au2 Cu2 N16, 4(Cl O4)'
_chemical_formula_sum            'C58 H48 Au2 Cl4 Cu2 N16 O16'
_chemical_formula_weight         1887.93
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
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2017-06-16 deposited with the CCDC.
2017-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.789(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.7148(14)
_cell_length_b                   13.6599(3)
_cell_length_c                   25.8961(8)
_cell_measurement_reflns_used    24334
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      1.57
_cell_volume                     14582.6(7)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.71.0.0 (STOE, 2016) X-Area X-Red32 1.63.2.0 (STOE, 2017)'
_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      110.15
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34765
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.092
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.806
_exptl_absorpt_correction_T_max  0.8074
_exptl_absorpt_correction_T_min  0.5625
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       plate
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.153
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         14227
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0952P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9443
_reflns_number_total             14227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04705c2.cif
_cod_data_source_block           cck333-1
_cod_database_code               7120554
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-O15 \\sim Cl4-O16 \\sim Cl4-O13 \\sim Cl4-O14
 with sigma of 0.02
 O15-O13 \\sim O16-O14 \\sim O15-O14 \\sim O16-O13 \\sim O15-O16 \\sim O13-O14
 with sigma of 0.04
 Cl2-O6 \\sim Cl2-O7 \\sim Cl2-O5 \\sim Cl2-O8
 with sigma of 0.02
 O6-O5 \\sim O7-O8 \\sim O6-O8 \\sim O7-O5 \\sim O6-O7 \\sim O5-O8
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim O13 \\sim O14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl2 \\sim O6 \\sim O7 \\sim O5 \\sim O8: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 Cl4, O15, O16, O13, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O6, O7, O5, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl4(0.5) O15(0.5) O16(0.5) O13(0.5) O14(0.5) Cl2(0.5) O6(0.5)
 O7(0.5) O5(0.5) O8(0.5)
6.a Free rotating group:
 Cl4(O15,O16,O13,O14), Cl2(O6,O7,O5,O8)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C15(H15a,H15b), C19(H19a,H19b), C33(H33a,H33b), C44(H44a,H44b),
 C48(H48a,H48b)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37),
 C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C50(H50), C51(H51),
  C52(H52), C55(H55), C56(H56), C57(H57), C58(H58)
;
_olex2_submission_special_instructions 'No special instructions were received'