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_1569965
_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, C8 H8 O2'
_chemical_formula_sum            'C53 H47 O11 P3'
_chemical_formula_weight         952.81
_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             2023-03-04
_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                88.789(5)
_cell_angle_beta                 83.362(5)
_cell_angle_gamma                88.235(5)
_cell_formula_units_Z            4
_cell_length_a                   9.4246(16)
_cell_length_b                   16.952(3)
_cell_length_c                   28.583(4)
_cell_measurement_reflns_used    3275
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      19.26
_cell_measurement_theta_min      2.37
_cell_volume                     4533.1(13)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2367
_diffrn_reflns_av_unetI/netI     0.1452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            102286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.152
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1551 before and 0.0994 after correction.
The Ratio of minimum to maximum transmission is 0.7741.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0148(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1227
_refine_ls_number_reflns         15938
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1753
_refine_ls_R_factor_gt           0.0823
_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^)+(0.0677P)^2^+8.6428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             15938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           q1_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_original_cell_volume        4533.0(12)
_cod_database_code               1569965
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.933
_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
 C7B-C1
 1.395 with sigma of 0.001
 C2A-C1
 1.395 with sigma of 0.001
 C02Z-C6 \\sim C02Z-C0
 with sigma of 0.02
 C11-C03D \\sim C4-C03D
 with sigma of 0.02
 C7-C6 \\sim C2-C0
 with sigma of 0.02
 C11-C7 \\sim C4-C2
 with sigma of 0.02
3. Rigid bond restraints
 C9, C10
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.006
 C4A, C02G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Uiso/Uaniso restraints and constraints
C02G \\sim C1 \\sim C2B \\sim C4B \\sim C6B \\sim C7B \\sim C6A \\sim C7A \\sim
C4A \\sim C2A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C2A \\sim C2B \\sim C1 \\sim C7A \\sim C7B: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
5. Rigid body (RIGU) restrains
 C6, C7, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C4B)=Sof(H4B)=Sof(C2B)=Sof(H2B)=Sof(H1B)=Sof(C7A)=Sof(H7A)=Sof(C6A)=
 Sof(H6A)=1-FVAR(1)
 Sof(H1A)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C4A)=Sof(H4A)=Sof(C2A)=
 Sof(H2A)=FVAR(1)
 Sof(H03A)=Sof(C4)=Sof(H4)=Sof(C0)=Sof(H0)=Sof(C2)=Sof(H2)=1-FVAR(2)
 Sof(H03D)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C11)=Sof(H11)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C010(H01G,H01H), C013(H01I,H01J), C016(H01K,H01L), C01D(H01A,H01B), C01M(H01C,
 H01D), C01N(H01E,H01F)
7.b Aromatic/amide H refined with riding coordinates:
 C023(H023), C02C(H02V), C02L(H02W), C02V(H02Z), C02K(H02), C02M(H1),
 C039(H039), C037(H037), C03E(H03E), C034(H034), C02N(H02N), C02X(H02X),
 C02Y(H02Y), C02U(H02U), C02H(H02H), C02R(H3), C03B(H03B), C032(H032),
 C03G(H03G), C033(H033), C4B(H4B), C2B(H2B), C1(H1B), C1(H1A), C7A(H7A),
 C6A(H6A), C031(H031), C035(H035), C036(H036), C038(H038), C03C(H03C),
 C03D(H03A), C03D(H03D), C03H(H03H), C4(H4), C0(H0), C2(H2), C6B(H6B), C7B(H7B),
  C3(H3A), C5(H5A), C8(H8A), C9(H9A), C10(H10A), C4A(H4A), C2A(H2A), C6(H6),
 C7(H7), C11(H11)
7.c Fitted hexagon refined as free rotating group:
 C01H(C023,C02C,C02L,C02V,C02K), C01V(C02M,C039,C037,C03E,C034), C025(C02N,
 C02X,C02Y,C02U,C02H), C02D(C02R,C03B,C032,C03G,C033), C02G(C4B,C2B,C1,C7A,C6A)
7.d Idealised Me refined as rotating group:
 C01C(H01M,H01N,H01O), C01E(H01P,H01Q,H01R), C01T(H01S,H01T,H01U), C021(H02A,
 H02B,H02C), C024(H12,H,HA), C027(H02D,H02E,H02F), C029(H02G,H02I,H02J),
 C02B(H10,HB,HC), C02E(H02K,H02L,H02M), C02F(H5,HD,HE), C02P(H02O,H02P,H02Q),
 C02Q(H02R,H02S,H02T), C02S(H8,HF,HG), C02T(H9,HH,HI)
;
_shelx_res_checksum              51576
_olex2_submission_special_instructions 'No special instructions were received'