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_7129284
_publ_section_title
;
 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         'C98 H58 Au6 F20 N4 P4, C4 H10 O'
_chemical_formula_sum            'C102 H68 Au6 F20 N4 O P4'
_chemical_formula_weight         3051.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-26 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0505(7)
_cell_length_b                   22.6822(7)
_cell_length_c                   13.1960(6)
_cell_measurement_reflns_used    25789
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.44
_cell_measurement_theta_min      1.51
_cell_volume                     5035.6(3)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.161.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.0.0 (STOE, 2020)
X-Area LANA 1.78.0.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.3 (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 1.89, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details
;
 226 frames, detector distance = 40 mm
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27656
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         1.507
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.857
_exptl_absorpt_correction_T_max  0.5359
_exptl_absorpt_correction_T_min  0.1581
_exptl_absorpt_correction_type   multi-scan
_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. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.524
_refine_diff_density_min         -2.661
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         13692
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0761P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9714
_reflns_number_total             13692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06034a2.cif
_cod_data_source_block           md183
_cod_database_code               7129284
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.197
_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. Uiso/Uaniso restraints and constraints
O \\sim C50 \\sim C51 \\sim C52 \\sim C53: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
3. Others
 Fixed Sof: O(0.5) C50(0.5) H50A(0.5) H50B(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 H51C(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C52(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37)
4.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              1537
_shelx_hkl_checksum              59975
_olex2_submission_special_instructions 'No special instructions were received'