;   () –; doi:10.1039/D3DT00850A

data_1569098
_journal_paper_doi               10.1039/D3DT00850A
_chemical_formula_moiety         '2(C30 H56 N6 P S2 Si), 1[C4H10O]'
_chemical_formula_sum            'C64 H122 N12 O P2 S4 Si2'
_chemical_formula_weight         1322.09
_chemical_name_systematic        MR-619
_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             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                90
_cell_angle_beta                 95.215(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8922(6)
_cell_length_b                   14.1605(5)
_cell_length_c                   22.8124(5)
_cell_measurement_reflns_used    22951
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.39
_cell_volume                     8007.8(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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      123.00
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 343 frames, detector distance = 130 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.417
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7104
_exptl_absorpt_correction_T_min  0.4116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens 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.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_size_rad          0.200
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         14465
_refine_ls_number_restraints     667
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+26.4594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9901
_reflns_number_total             14465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00850a2.cif
_cod_data_source_block           5b
_cod_database_code               1569098
_shelx_shelxl_version_number     2014/7
_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
2. Restrained distances
 C22T-C21T = C21A-C22A = C20A-C21A = C20A-C19A = C17A-C18T = C17A-C18A = C17A-
 C16A = C7-C6 = C6-C5 = C11-C10
 1.5 with sigma of 0.01
 C21T-C20A
 1.5 with sigma of 0.01
 C9-C8
 1.5 with sigma of 0.01
 C20A-C19A
 1.5 with sigma of 0.01
 C17A-C18A
 1.5 with sigma of 0.01
 C9S-C8
 1.5 with sigma of 0.01
 C19A-C20T = C20T-C21T
 1.5 with sigma of 0.01
 C10S-C9S = C10S-C11S
 1.5 with sigma of 0.001
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H19C)=Sof(H19D)=Sof(C20T)=Sof(H20C)=Sof(H20D)=Sof(C21T)=Sof(H21C)=
 Sof(H21D)=Sof(C22T)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(H17C)=Sof(H17D)=Sof(C18T)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(H8BE)=Sof(H8BF)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(C10S)=Sof(H10E)=
 Sof(H10F)=Sof(C11S)=Sof(H11G)=Sof(H11H)=Sof(H11I)=1-FVAR(3)
 Sof(H8AC)=Sof(H8AD)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10C)=Sof(H10D)=
 Sof(C11)=Sof(H11D)=Sof(H11E)=Sof(H11F)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8AC,H8AD), C8(H8BE,H8BF), C9(H9A,
 H9B), C9S(H9SA,H9SB), C10(H10C,H10D), C10S(H10E,H10F), C15(H15C,H15D),
 C16(H16C,H16D), C17(H17E,H17F), C19(H19E,H19F), C20(H20E,H20F), C21(H21E,H21F),
  C23(H23C,H23D), C25(H25C,H25D), C27(H27C,H27D), C29(H29C,H29D), C4A(H4AA,
 H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB),
 C10A(H10A,H10B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C17A(H17C,
 H17D), C19A(H19A,H19B), C19A(H19C,H19D), C20A(H20A,H20B), C20T(H20C,H20D),
 C21A(H21A,H21B), C21T(H21C,H21D), C23A(H23A,H23B), C25A(H25A,H25B), C27A(H27A,
 H27B), C29A(H29A,H29B)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11D,H11E,H11F), C11S(H11G,H11H,H11I), C18(H18G,H18H,
 H18I), C22(H22G,H22H,H22I), C24(H24D,H24E,H24F), C26(H26D,H26E,H26F), C28(H28D,
 H28E,H28F), C30(H30D,H30E,H30F), C7A(H7AA,H7AB,H7AC), C11A(H11A,H11B,H11C),
 C18A(H18A,H18B,H18C), C18T(H18D,H18E,H18F), C22A(H22A,H22B,H22C), C22T(H22D,
 H22E,H22F), C24A(H24A,H24B,H24C), C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C),
 C30A(H30A,H30B,H30C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91894
_shelx_fab_checksum              36724
_olex2_submission_special_instructions 'No special instructions were received'