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_7120556
_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         '2(Cl), C29 H26 N8'
_chemical_formula_sum            'C29 H26 Cl2 N8'
_chemical_formula_weight         557.48
_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   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                92.009(6)
_cell_angle_beta                 96.335(6)
_cell_angle_gamma                92.319(6)
_cell_formula_units_Z            4
_cell_length_a                   11.9504(9)
_cell_length_b                   12.7279(10)
_cell_length_c                   17.9011(13)
_cell_measurement_reflns_used    11334
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      1.60
_cell_volume                     2701.8(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.974
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20969
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.221
_diffrn_reflns_theta_min         1.602
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9638
_exptl_absorpt_correction_T_min  0.9110
_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    1.370
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0391P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6315
_reflns_number_total             10600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04705c2.cif
_cod_data_source_block           cck266-4
_cod_database_code               7120556
_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.a Secondary CH2 refined with riding coordinates:
 C15'(H15A,H15B), C4'(H4'A,H4'B), C19'(H19A,H19B), C15(H15C,H15D), C19(H19C,
 H19D), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C1'(H1'), C16'(H16'), C23'(H23'), C17'(H17'), C2'(H2'), C21'(H21'), C6'(H6'),
 C7'(H7'), C13'(H13'), C12'(H12'), C8'(H8'), C11'(H11'), C3'(H3'), C18'(H18'),
 C22'(H22'), C14'(H14'), C26'(H26'), C29'(H29'), C18(H18), C21(H21), C16(H16),
 C11(H11), C26(H26), C12(H12), C1(H1), C3(H3), C17(H17), C6(H6), C14(H14),
 C13(H13), C8(H8), C2(H2), C23(H23), C27(H27), C29(H29), C7(H7), C22(H22),
 C28(H28), C28'(H28'), C27'(H27')
;
_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'