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_7120555
_publ_section_title
;
 Defined tetranuclear coinage metal chains
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04705C
_journal_year                    2017
_chemical_formula_moiety         'C58 H48 Ag2 Au2 N16, 4(Cl O4), C2 H3 N'
_chemical_formula_sum            'C60 H51 Ag2 Au2 Cl4 N17 O16'
_chemical_formula_weight         2017.65
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-06-16 deposited with the CCDC.
2017-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                91.502(3)
_cell_angle_beta                 101.697(3)
_cell_angle_gamma                107.160(3)
_cell_formula_units_Z            4
_cell_length_a                   14.6489(5)
_cell_length_b                   19.5901(7)
_cell_length_c                   26.9914(10)
_cell_measurement_reflns_used    38214
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      1.49
_cell_volume                     7216.6(5)
_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      210
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            54370
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.128
_diffrn_reflns_theta_min         1.521
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    4.812
_exptl_absorpt_correction_T_max  0.5192
_exptl_absorpt_correction_T_min  0.1831
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       prism
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1851
_refine_ls_number_reflns         28168
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18905
_reflns_number_total             28168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04705c2.cif
_cod_data_source_block           cck334-1_sq
_cod_database_code               7120555
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1a-N34A
 1.456 with sigma of 0.01
 C1b-N34A
 2.593 with sigma of 0.02
 Cl8A-O32A \\sim Cl8A-O30A \\sim Cl8A-O29A \\sim Cl8A-O31A
 with sigma of 0.02
 O32A-O29A \\sim O30A-O31A \\sim O32A-O31A \\sim O30A-O29A \\sim O32A-O30A
\\sim O29A-O31A
 with sigma of 0.04
3. Rigid bond restraints
 N19, C67, C66, C64, C65, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl6 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim Cl4 \\sim O13 \\sim O14 \\sim
O15 \\sim O16: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Cl8A \\sim O32A \\sim O30A \\sim O29A \\sim O31A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
N34A \\sim C1a \\sim C1b: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O29A) \\sim Ueq, Uanis(O31A) \\sim Ueq, Uanis(Cl8A) \\sim Ueq,
Uanis(O30A) \\sim Ueq, Uanis(O32A) \\sim Ueq: with sigma of 0.0005 and sigma
for terminal atoms of 0.001
5. Rigid body (RIGU) restrains
 Cl8A, O32A, O30A, O29A, O31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N34A, C1a, C1b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl8A(0.5) O32A(0.5) O30A(0.5) O29A(0.5) O31A(0.5) Cl8B(0.5)
 O29B(0.5) O30B(0.5) O31B(0.5) O32B(0.5) N34B(0.5) C119(0.5) H11d(0.5)
 H11e(0.5) H11f(0.5) C120(0.5) N34A(0.5) C1a(0.5) C1b(0.5) H11g(0.5) H11h(0.5)
 H11i(0.5)
7.a Riding coordinates:
 C1b(H11g,H11h,H11i)
7.b Free rotating group:
 Cl8A(O32A,O30A,O29A,O31A), N34A(C1a,C1b)
7.c Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C15(H15a,H15b), C33(H33a,H33b), C19(H19a,H19b), C48(H48a,H48b),
 C44(H44a,H44b), C73(H73a,H73b), C77(H77a,H77b), C102(H10a,H10b), C106(H10c,
 H10d), C62(H62a,H62b), C91(H91a,H91b)
7.d Aromatic/amide H refined with riding coordinates:
 C32(H32), C7(H7), C11(H11), C3(H3), C14(H14), C6(H6), C18(H18), C42(H42),
 C31(H31), C47(H47), C13(H13), C55(H55), C41(H41), C12(H12), C43(H43), C29(H29),
  C37(H37), C35(H35), C36(H36), C57(H57), C50(H50), C22(H22), C8(H8), C40(H40),
 C46(H46), C2(H2), C56(H56), C17(H17), C52(H52), C21(H21), C51(H51), C28(H28),
 C58(H58), C23(H23), C27(H27), C26(H26), C84(H84), C105(H105), C76(H76),
 C113(H113), C104(H104), C87(H87), C85(H85), C79(H79), C99(H99), C98(H98),
 C100(H100), C93(H93), C116(H116), C69(H69), C60(H60), C101(H101), C89(H89),
 C108(H108), C109(H109), C61(H61), C94(H94), C90(H90), C71(H71), C114(H114),
 C115(H115), C110(H110), C72(H72), C66(H66), C64(H64), C65(H65), C81(H81),
 C75(H75), C80(H80), C86(H86), C95(H95), C70(H70)
7.e Idealised Me refined as rotating group:
 C117(H11a,H11b,H11c), C119(H11d,H11e,H11f)
;
_shelx_res_checksum              77766
_shelx_fab_checksum              48755
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'