Host-guest system of a phosphorylated macrocycle assisting structure determination of oily molecules in single-crystal form.
Jiao, Jianmin; Li, Heng; Xie, Wang; Zhao, Yue; Lin, Chen; Jiang, Juli; Wang, Leyong; Chemical science 14 (2023) 11402–11409; doi:10.1039/d3sc02995f

data_1569969
_publ_section_title
;
 Host-guest system of a phosphorylated macrocycle assisting structure
 determination of oily molecules in single-crystal form.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              11402
_journal_page_last               11409
_journal_paper_doi               10.1039/d3sc02995f
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H39 O9 P3, 2(C3 H5 Cl O)'
_chemical_formula_sum            'C51 H49 Cl2 O11 P3'
_chemical_formula_weight         1001.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-03-27 deposited with the CCDC.	2023-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.006(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9718(4)
_cell_length_b                   17.5666(8)
_cell_length_c                   29.7758(13)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      68.108
_cell_measurement_theta_min      2.921
_cell_volume                     4692.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            169403
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.515
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0937 after correction.
The Ratio of minimum to maximum transmission is 0.6700.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 7961 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.108(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         17036
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0401
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                16824
_reflns_number_total             17036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569969
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6646(11)
 0.3354(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C5-C12
 1.4 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H3BC)=Sof(H3BD)=Sof(Cl6)=1-FVAR(1)
 Sof(Cl1)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C10(H10), C19(H19), C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C59(H59A,H59B), C65(H65A,H65B), C66(H66A,H66B), C1(H1A,H1B),
 C2(H2A,H2B), C11(H11D,H11E), C13(H13A,H13B), C15(H15A,H15B), C9(H9A,H9B),
 C16(H16A,H16B), C18(H18A,H18B), C3(H3AA,H3AB), C3(H3BC,H3BD), C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C43(H43), C47(H47), C54(H54), C89(H89), C67(H67), C62(H62),
 CXF(HXF), C71(H71), C76(H76), C77(H77), C79(H79), C83(H83), C84(H84), C88(H88),
  C101(H101), C104(H104), C107(H107), C109(H109), C111(H111), C114(H114),
 C119(H119), C124(H124), C128(H128), C130(H130), C132(H132), C137(H137),
 C138(H138), C140(H140), C142(H142)
6.d Fitted hexagon refined as free rotating group:
 C55(C54,C89,C67,C62,CXF)
6.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C60(H60A,H60B,
 H60C), C68(H68A,H68B,H68C), C75(H75A,H75B,H75C), C91(H91A,H91B,H91C), C97(H97A,
 H97B,H97C), C100(H10A,H10B,H10C), C103(H10G,H10H,H10I), C105(H10D,H10E,H10F),
 C110(H11A,H11B,H11C)
;
_shelx_res_checksum              12374
_olex2_submission_special_instructions 'No special instructions were received'