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_1569957
_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_formula_moiety         'C45 H39 O9 P3, C11 H14 O2'
_chemical_formula_sum            'C56 H53 O11 P3'
_chemical_formula_weight         994.89
_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   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                114.852(3)
_cell_angle_beta                 90.936(3)
_cell_angle_gamma                105.208(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4775(4)
_cell_length_b                   16.7701(8)
_cell_length_c                   17.2391(9)
_cell_measurement_reflns_used    6475
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      46.705
_cell_measurement_theta_min      2.483
_cell_volume                     2374.0(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_unetI/netI     0.1163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32048
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.412
_diffrn_reflns_theta_min         1.316
_diffrn_source_current           2.86
_diffrn_source_power             0.1993134
_diffrn_source_voltage           69.69
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1321 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.8247.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         8729
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0822P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4689
_reflns_number_total             8729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           1a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569957
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.974
_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. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(H01Y)=Sof(C01V)=Sof(H1)=Sof(C01X)=Sof(H3)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=1-FVAR(1)
 Sof(H01X)=Sof(C01O)=Sof(H01Z)=Sof(C01Q)=Sof(H01)=Sof(C01W)=Sof(H2)=Sof(C01Y)=
 Sof(H4)=FVAR(1)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(C4)=Sof(H4A)=Sof(C2)=Sof(H2A)=
 Sof(O2)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(2)
 Sof(C5)=Sof(H5A)=Sof(C8)=Sof(H8)=Sof(C3)=Sof(C7)=Sof(H7)=Sof(C6)=Sof(H6A)=
 Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00T(H00C,H00D), C00Z(H00H,H00I), C01B(H5,H), C01G(H6,HA)
5.b Aromatic/amide H refined with riding coordinates:
 C018(H018), C019(H019), C01A(H01M), C01C(H01N), C01D(H01O), C01E(H01P),
 C11(H11), C10(H10), C4(H4A), C2(H2A), C5(H5A), C8(H8), C7(H7), C6(H6A),
 C01J(H01T), C01K(H01U), C01L(H01V), C01M(H01W), C01N(H01X), C01N(H01Y),
 C01O(H01Z), C01Q(H01), C01V(H1), C01W(H2), C01X(H3), C01Y(H4), C13(H13),
 C14(H14)
5.c Fitted hexagon refined as free rotating group:
 C01H(C11,C10,C9,C4,C2)
5.d Idealised Me refined as rotating group:
 C00W(H00E,H00F,H00G), C012(H01A,H01B,H01C), C015(H01D,H01E,H01F), C016(H01G,
 H01H,H01I), C017(H01J,H01K,H01L), C01F(H01Q,H01R,H01S), C01I(H9,HB,HC),
 C12(H12A,H12B,H12C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              56246
_olex2_submission_special_instructions 'No special instructions were received'