Tetra- and hexanuclear string complexes of the coinage metals
Dahlen, Milena; Seifert, Tim P.; Lebedkin, Sergei; Gamer, Michael T.; Kappes, Manfred M.; Roesky, Peter W.; Chemical Communications  (2021) –; doi:10.1039/D1CC06034A

data_7129283
_publ_section_title
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 Tetra- and hexanuclear string complexes of the coinage metals
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06034A
_journal_year                    2021
_chemical_formula_moiety
'C92 H80 Au2 Cu2 N4 P4, 0.5(C4 H8 O), 0.5(C5 H12)'
_chemical_formula_sum            'C96.5 H90 Au2 Cu2 N4 O0.5 P4'
_chemical_formula_weight         1958.61
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-26 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   35.0732(3)
_cell_length_b                   35.0732(3)
_cell_length_c                   39.2104(4)
_cell_measurement_reflns_used    120689
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      1.16
_cell_volume                     41771.8(7)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 203 frames, detector distance = 135 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            74831
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.342
_diffrn_reflns_theta_min         1.848
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current           40mA
_diffrn_source_power             2kW
_diffrn_source_voltage           50kV
_exptl_absorpt_coefficient_mu    3.717
_exptl_absorpt_correction_T_max  0.5828
_exptl_absorpt_correction_T_min  0.3493
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17586
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0431P)^2^+200.5224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7629
_reflns_number_total             8416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06034a2.cif
_cod_data_source_block           md143
_cod_original_cell_volume        41771.7(8)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C96.50 H90 Au2 Cu2 N4 O0.50 P4'
_cod_database_code               7129283
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.260
_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
 C51A-C50A \\sim C50A-C49A \\sim C49A-C48A
 with sigma of 0.02
 O1B-C51A \\sim O1B-C48A
 with sigma of 0.02
 O1B-C50A \\sim O1B-C49A
 with sigma of 0.04
 C50A-C48A \\sim C51A-C49A
 with sigma of 0.04
 C48B-C49B \\sim C49B-C50B \\sim C50B-C51B
 with sigma of 0.02
 O1A-C48B \\sim O1A-C51B
 with sigma of 0.02
 O1A-C49B \\sim O1A-C50B
 with sigma of 0.04
 C49B-C51B \\sim C48B-C50B
 with sigma of 0.04
 C52A-C53A \\sim C53A-C54A \\sim C54A-C55A \\sim C55A-C56A
 with sigma of 0.02
 C52A-C54A \\sim C54A-C56A \\sim C53A-C55A
 with sigma of 0.04
 C52B-C53B \\sim C53B-C54B \\sim C54B-C55B \\sim C55B-C56B
 with sigma of 0.02
 C52B-C54B \\sim C54B-C56B \\sim C53B-C55B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C56B \\sim C55B \\sim C54B \\sim C53B \\sim C52B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C48A \\sim C49A \\sim C50A \\sim C51A \\sim O1B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C51B \\sim C50B \\sim C49B \\sim C48B \\sim O1A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O1A(0.125) C48B(0.125) H48A(0.125) H48B(0.125) C49B(0.125)
 H49A(0.125) H49B(0.125) C50B(0.125) H50A(0.125) H50B(0.125) C51B(0.125)
 H51A(0.125) H51B(0.125) O1B(0.125) C48A(0.125) H48C(0.125) H48D(0.125)
 C49A(0.125) H49C(0.125) H49D(0.125) C50A(0.125) H50C(0.125) H50D(0.125)
 C51A(0.125) H51C(0.125) H51D(0.125) C52A(0.125) H52A(0.125) H52B(0.125)
 H52C(0.125) C53A(0.125) H53A(0.125) H53B(0.125) C54A(0.125) H54A(0.125)
 H54B(0.125) C55A(0.125) H55A(0.125) H55B(0.125) C56A(0.125) H56A(0.125)
 H56B(0.125) H56C(0.125) C52B(0.125) H52D(0.125) H52E(0.125) H52F(0.125)
 C53B(0.125) H53C(0.125) H53D(0.125) C54B(0.125) H54C(0.125) H54D(0.125)
 C55B(0.125) H55C(0.125) H55D(0.125) C56B(0.125) H56D(0.125) H56E(0.125)
 H56F(0.125)
5.a Free rotating group:
 O1A(C48B,C49B,C50B,C51B), O1B(C48A,C49A,C50A,C51A), C52A(C53A,C54A,C55A,C56A),
  C52B(C53B,C54B,C55B,C56B)
5.b Secondary CH2 refined with riding coordinates:
 C48B(H48A,H48B), C49B(H49A,H49B), C50B(H50A,H50B), C51B(H51A,H51B), C48A(H48C,
 H48D), C49A(H49C,H49D), C50A(H50C,H50D), C51A(H51C,H51D), C53A(H53A,H53B),
 C54A(H54A,H54B), C55A(H55A,H55B), C53B(H53C,H53D), C54B(H54C,H54D), C55B(H55C,
 H55D)
5.c Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C56A(H56A,H56B,H56C), C52B(H52D,H52E,H52F), C56B(H56D,
 H56E,H56F)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C43(H43)
5.e Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
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_shelx_res_checksum              1210
_shelx_hkl_checksum              3305
_olex2_submission_special_instructions 'No special instructions were received'