;   () –; doi:10.1039/D3DT00850A

data_1569099
_journal_paper_doi               10.1039/D3DT00850A
_chemical_formula_moiety         'C60 H113 K N12 P2 S4 Si2, 1.5[C4H10O]'
_chemical_formula_sum            'C66 H128 K N12 O1.5 P2 S4 Si2'
_chemical_formula_weight         1399.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                64.358(2)
_cell_angle_beta                 77.924(2)
_cell_angle_gamma                85.049(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1993(6)
_cell_length_b                   17.4995(7)
_cell_length_c                   18.3108(8)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.14
_cell_measurement_theta_min      3.18
_cell_volume                     4011.0(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128554
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.743
_diffrn_reflns_theta_min         4.231
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.569
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1499 before and 0.0851 after correction.
The Ratio of minimum to maximum transmission is 0.7320.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         14478
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0587P)^2^+1.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13019
_reflns_number_total             14478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00850a2.cif
_cod_data_source_block           4b
_cod_original_formula_sum        'C66 H128 K N12 O1.50 P2 S4 Si2'
_cod_database_code               1569099
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 P2-H2
 1.5 with sigma of 0.02
 P1-H1
 1.5 with sigma of 0.02
3. Others
 Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(C10S)=Sof(H10C)=
 Sof(H10D)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Sof(H47C)=Sof(H47D)=Sof(C48S)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(2)
 Fixed Sof: H2(0.5) H1(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C8S(H8SA,H8SB), C9(H9A,
 H9B), C9S(H9SA,H9SB), C10(H10A,H10B), C10S(H10C,H10D), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C47(H47C,H47D),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,
 H55B), C57(H57A,H57B), C59(H59A,H59B)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C11(H11D,H11E,H11F), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C),
 C48(H48A,H48B,H48C), C48S(H48D,H48E,H48F), C52(H52A,H52B,H52C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47342
_shelx_fab_checksum              170
_olex2_submission_special_instructions 'No special instructions were received'