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_1569964
_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, C7 H8'
_chemical_formula_sum            'C52 H47 O9 P3'
_chemical_formula_weight         908.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 90.6240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1991(3)
_cell_length_b                   10.1623(2)
_cell_length_c                   28.6677(6)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      5.35
_cell_volume                     4719.00(16)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.999
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            169107
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.278
_diffrn_reflns_theta_min         3.083
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  0.5849
_exptl_absorpt_correction_T_min  0.5194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1146 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.8880.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       needle
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8638
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0678P)^2^+3.4549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8270
_reflns_number_total             8638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           cu_20220603_xw_jjm311_0m_sq
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569964
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.688
_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
 C2-C4
 1.4 with sigma of 0.01
 C4-C11
 1.4 with sigma of 0.01
 C8-C6
 1.4 with sigma of 0.01
 C7A-C3 \\sim C7B-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim C4 \\sim C11 \\sim C10 \\sim C9 \\sim C8: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
4. Others
 Sof(H1B)=Sof(H2B)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(1)
 Sof(H1A)=Sof(H2A)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=
 Sof(H7BC)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00L(H00C,H00D), C00R(H00E,H00F)
5.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C011(H011), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C019(H019), C01B(H01G), C01C(H01H), C01E(H01L), C01G(H01P),
 C01H(H01Q), C01J(H01U), C01L(H01Y), C1(H1B), C1(H1A), C2(H2B), C2(H2A), C4(H4),
  C6(H6), C8(H8), C9(H9), C10(H10), C11(H11)
5.c Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01D(H01I,H01J,H01K), C01F(H01M,
 H01N,H01O), C01I(H01R,H01S,H01T), C01K(H01V,H01W,H01X), C7B(H7BA,H7BB,H7BC),
 C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              57828
_shelx_fab_checksum              38589
_olex2_submission_special_instructions 'No special instructions were received'