Triple-decker complexes incorporating three distinct deck architectures
Sun, Xiaofei; Singh, Akhil Kumar; Yadav, Ravi; Jin, Da; Haimerl, Maria; Scheer, Manfred; Roesky, Peter W.; Chemical Communications  (2022) –; doi:10.1039/D1CC06182H

data_7129403
_publ_section_title
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 Triple-decker complexes incorporating three distinct deck architectures
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06182H
_journal_year                    2022
_chemical_formula_moiety         'C84 H126 As10 Fe2 Li4 O2 Pb2 Si4, 3(C6 H6)'
_chemical_formula_sum            'C102 H144 As10 Fe2 Li4 O2 Pb2 Si4'
_chemical_formula_weight         2817.56
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.349(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1239(5)
_cell_length_b                   19.7028(2)
_cell_length_c                   24.2819(5)
_cell_measurement_reflns_used    76485
_cell_measurement_temperature    150
_cell_measurement_theta_max      64.24
_cell_measurement_theta_min      3.18
_cell_volume                     11474.7(4)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (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 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 EIGER4M
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
 1099 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70573
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.524
_diffrn_reflns_theta_min         3.176
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_type              'Ga Metaljet D2'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    7.736
_exptl_absorpt_correction_T_max  0.1754
_exptl_absorpt_correction_T_min  0.0459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5544
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1227
_refine_ls_number_reflns         26475
_refine_ls_number_restraints     648
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+1.7330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0892
_reflns_d_resolution_high        0.756
_reflns_d_resolution_low         12.111
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              15
_reflns_limit_h_min              -34
_reflns_limit_k_max              23
_reflns_limit_k_min              -26
_reflns_limit_l_max              31
_reflns_limit_l_min              -31
_reflns_number_gt                20697
_reflns_number_total             26475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06182h2.cif
_cod_data_source_block           xf-366-d-neu
_cod_database_code               7129403
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.685
_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. Rigid bond restraints
 C1A, C1B, C1C, C97B, C98B, C99B, H35C, C91A, C91B, C92A, C92B, C93A, C93B,
 C94A, C94B, C95A, C95B, C96A, C96B, C97A, C98A, C99A, C100, C101, C102
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C97B \\sim C98B \\sim C99B \\sim C91A \\sim C91B
\\sim C92A \\sim C92B \\sim C93A \\sim C93B \\sim C94A \\sim C94B \\sim C95A
\\sim C95B \\sim C96A \\sim C96B \\sim C97A \\sim C98A \\sim C99A \\sim C100
\\sim C101 \\sim C102: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2.5A
4. Others
 Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C97A)=
 Sof(H97A)=Sof(C98A)=Sof(H98A)=Sof(C99A)=Sof(H99A)=1-FVAR(1)
 Sof(C98B)=Sof(H98B)=Sof(C99B)=Sof(H99B)=Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=
 Sof(C1C)=Sof(H1C)=Sof(C97B)=Sof(H97B)=FVAR(1)
 Sof(C94A)=Sof(H94A)=Sof(C95A)=Sof(H95A)=Sof(C96A)=Sof(H96A)=Sof(C91A)=
 Sof(H91A)=Sof(C92A)=Sof(H92A)=Sof(C93A)=Sof(H93A)=1-FVAR(2)
 Sof(C94B)=Sof(H94B)=Sof(C95B)=Sof(H95B)=Sof(C96B)=Sof(H96B)=Sof(C91B)=
 Sof(H91B)=Sof(C92B)=Sof(H92B)=Sof(C93B)=Sof(H93B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
5.b Aromatic/amide H refined with riding coordinates:
 C98B(H98B), C99B(H99B), C1A(H1A), C1B(H1B), C1C(H1C), C97B(H97B), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C85(H85), C86(H86), C87(H87), C88(H88),
  C89(H89), C90(H90), C94A(H94A), C95A(H95A), C96A(H96A), C91A(H91A),
 C92A(H92A), C93A(H93A), C94B(H94B), C95B(H95B), C96B(H96B), C91B(H91B),
 C92B(H92B), C93B(H93B), C100(H100), C101(H101), C102(H102), C97A(H97A),
 C98A(H98A), C99A(H99A)
5.c Fitted hexagon refined as free rotating group:
 C98B(C99B,C1A,C1B,C1C,C97B), C94A(C95A,C96A,C91A,C92A,C93A), C94B(C95B,C96B,
 C91B,C92B,C93B), C100(C101,C102,C97A,C98A,C99A)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C76(H76A,H76B,H76C), C77(H77A,
 H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              77472
_shelx_hkl_checksum              58698
_olex2_submission_special_instructions 'No special instructions were received'