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_7129402
_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         'C32 H48 Li O P Si2'
_chemical_formula_sum            'C32 H48 Li O P Si2'
_chemical_formula_weight         542.79
_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                 99.295(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8956(12)
_cell_length_b                   23.8229(9)
_cell_length_c                   12.4303(7)
_cell_measurement_reflns_used    23179
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.46
_cell_volume                     6398.7(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_details
;
 367 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'single reflection optic'
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33188
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.248
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_type              'Xenocs Genix3D microfocus'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.9601
_exptl_absorpt_correction_T_min  0.3746
_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, "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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.652
_exptl_crystal_size_mid          0.363
_exptl_crystal_size_min          0.147
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         15740
_refine_ls_number_restraints     601
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1090P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1848
_reflns_d_resolution_high        0.705
_reflns_d_resolution_low         9.996
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              17
_reflns_limit_h_min              -10
_reflns_limit_k_max              30
_reflns_limit_k_min              -31
_reflns_limit_l_max              29
_reflns_limit_l_min              -28
_reflns_number_gt                10490
_reflns_number_total             15740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06182h2.cif
_cod_data_source_block           xf375b
_cod_database_code               7129402
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.890
_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
 O1A-C32A \\sim O1B-C32B
 with sigma of 0.02
 O1A-C29A \\sim O1B-C29B
 with sigma of 0.02
 C32A-C29A \\sim C32B-C29B
 with sigma of 0.04
 O1A-Li1 \\sim O1B-Li1
 with sigma of 0.02
 C31A-C29A \\sim C31B-C29B
 with sigma of 0.04
 C31A-C30A \\sim C31B-C30B
 with sigma of 0.02
 C31A-C32A \\sim C31B-C32B
 with sigma of 0.02
 C30A-C32A \\sim C30B-C32B
 with sigma of 0.04
 C30A-C29A \\sim C30B-C29B
 with sigma of 0.02
 C32A-Li1 \\sim C32B-Li1
 with sigma of 0.04
 O1A-C31A \\sim O1B-C31B
 with sigma of 0.04
 O1A-C30A \\sim O1B-C30B
 with sigma of 0.04
 C29A-Li1 \\sim C29B-Li1
 with sigma of 0.04
 C64A-Li2 \\sim C64B-Li2
 with sigma of 0.04
 C62A-Li2 \\sim C62B-Li2
 with sigma of 0.04
 C63A-C62A \\sim C32-C62B
 with sigma of 0.04
 C61A-C64A \\sim C61B-C64B
 with sigma of 0.04
 C63A-C61A \\sim C32-C61B
 with sigma of 0.04
 C63A-C64A \\sim C32-C64B
 with sigma of 0.04
 C61A-Li2 \\sim C61B-Li2
 with sigma of 0.04
 C62A-C64A \\sim C62B-C64B
 with sigma of 0.04
 O2A-C63A \\sim O2B-C32
 with sigma of 0.04
 O2A-C61A \\sim O2B-C61B
 with sigma of 0.04
 O2A-C62A \\sim O2B-C62B
 with sigma of 0.04
 O2A-C64A \\sim O2B-C64B
 with sigma of 0.04
 O2A-Li2 \\sim O2B-Li2
 with sigma of 0.04
 C61A-C62A \\sim C61B-C62B
 with sigma of 0.02
3. Rigid bond restraints
 O1A, O1B, C29A, C29B, C30A, C30B, C31A, C31B, C32A, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2A, O2B, C32, C61A, C61B, C62A, C62B, C63A, C64A, C64B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1A \\sim O1B \\sim C29A \\sim C29B \\sim C30A \\sim C30B \\sim C31A \\sim C31B
\\sim C32A \\sim C32B: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2.5A
O2A \\sim O2B \\sim C32 \\sim C61A \\sim C61B \\sim C62A \\sim C62B \\sim C63A
\\sim C64A \\sim C64B: within 2.5A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2.5A
5. Others
 Sof(O1B)=Sof(C29B)=Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30C)=Sof(H30D)=
 Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(O1A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(O2B)=Sof(C32)=Sof(H32E)=Sof(H32F)=Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=
 Sof(H62C)=Sof(H62D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=1-FVAR(2)
 Sof(O2A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=Sof(H62B)=
 Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(C64A)=Sof(H64A)=Sof(H64B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C29B(H29C,H29D), C30A(H30A,H30B), C30B(H30C,H30D), C31A(H31A,
 H31B), C31B(H31C,H31D), C32A(H32A,H32B), C32B(H32C,H32D), C32(H32E,H32F),
 C61A(H61A,H61B), C61B(H61C,H61D), C62A(H62A,H62B), C62B(H62C,H62D), C63A(H63A,
 H63B), C64A(H64A,H64B), C64B(H64C,H64D)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
6.c 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), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              28868
_shelx_hkl_checksum              8000
_olex2_submission_special_instructions 'No special instructions were received'