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_1569954
_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, C6 H12 O2'
_chemical_formula_sum            'C51 H51 O11 P3'
_chemical_formula_weight         932.82
_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             2023-01-01
_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                61.976(2)
_cell_angle_beta                 88.724(2)
_cell_angle_gamma                88.902(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6814(5)
_cell_length_b                   15.7995(11)
_cell_length_c                   16.5384(11)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.47
_cell_volume                     2232.5(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75399
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.448
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1584 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.9360.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10172
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0717P)^2^+1.3839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8698
_reflns_number_total             10172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           q1
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569954
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. 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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-C01P
 1.3 with sigma of 0.01
3. Others
 Sof(HA)=Sof(HB)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(O1)=Sof(H1A)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5)=1-FVAR(1)
 Sof(O00Q)=Sof(H00Q)=Sof(H1)=Sof(H)=Sof(C01Q)=Sof(H2)=Sof(C01R)=Sof(H3)=
 Sof(HE)=Sof(C01S)=Sof(H4)=Sof(HF)=Sof(HG)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C01Q(H2), C5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00P(H00C,H00D), C00U(H00E,H00F), C01H(H1,H), C01H(HA,HB),
 C01R(H3,HE), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C014(H014), C015(H015), C016(H016), C018(H018), C01A(H01J), C01B(H01K),
 C01C(H01L), C01D(H01M), C01E(H01N), C01G(H01R), C01I(H01S), C01K(H01W),
 C01L(H01X), C01M(H01Y), C01N(H01Z)
4.d Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C017(H01D,H01E,H01F), C019(H01G,H01H,H01I), C01F(H01O,
 H01P,H01Q), C01J(H01T,H01U,H01V), C01O(H01,HC,HD), C01S(H4,HF,HG), C1(H1AA,
 H1AB,H1AC), C1(H1BD,H1BE,H1BF), C2(H2A,H2B,H2C)
4.e Idealised tetrahedral OH refined as rotating group:
 O00Q(H00Q), O1(H1A)
;
_shelx_res_checksum              65989
_olex2_submission_special_instructions 'No special instructions were received'