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_7120553
_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         'C29 H24 Au2 Cl2 N8'
_chemical_formula_sum            'C29 H24 Au2 Cl2 N8'
_chemical_formula_weight         949.39
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-20
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   10.5556(6)
_cell_length_b                   28.004(2)
_cell_length_c                   44.889(3)
_cell_measurement_reflns_used    6495
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      1.71
_cell_volume                     13269.1(15)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            8670
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.173
_diffrn_reflns_theta_min         1.714
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    9.027
_exptl_absorpt_correction_T_max  0.3579
_exptl_absorpt_correction_T_min  0.2233
_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    1.901
_exptl_crystal_description       prism
_exptl_crystal_F_000             7136
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0454P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1907
_reflns_number_total             2964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04705c2.cif
_cod_data_source_block           cck274-5
_cod_database_code               7120553
_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. Others
 Fixed Sof: H15A(0.5) H15B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C15(H15A,H15B)
3.b 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)
;
_shelx_res_checksum              2321
_shelx_fab_checksum              57758
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop using mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'