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_1569976
_publ_section_title
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 Host-guest system of a phosphorylated macrocycle assisting structure
 determination of oily molecules in single-crystal form.
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_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(C5 H12 O)'
_chemical_formula_sum            'C55 H63 O11 P3'
_chemical_formula_weight         992.96
_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                 116.6350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5745(4)
_cell_length_b                   10.2015(2)
_cell_length_c                   24.3748(4)
_cell_measurement_reflns_used    9094
_cell_measurement_temperature    198.0
_cell_measurement_theta_max      68.104
_cell_measurement_theta_min      3.917
_cell_volume                     5017.68(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      198.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            208069
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.277
_diffrn_reflns_theta_min         2.189
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1186 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.8211.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 7520 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         17954
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0657P)^2^+1.9703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                17034
_reflns_number_total             17954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           111
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_original_cell_volume        5017.67(16)
_cod_database_code               1569976
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.785
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 H02K-H02Q
 2.2 with sigma of 0.02
 C16-C17
 1.54 with sigma of 0.02
 C9-C24A \\sim C9-C24B
 with sigma of 0.02
 C24A-C20A \\sim C24B-C20B
 with sigma of 0.02
 C21-C20A \\sim C21-C20B
 with sigma of 0.02
3. Others
 Sof(H9B)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C24B)=Sof(H24A)=Sof(H24B)=1-FVAR(1)
 Sof(H9A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C24A)=Sof(H24C)=Sof(H24D)=
 Sof(C20A)=Sof(H20C)=Sof(H20D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9B), C9(H9A), C3(H3A), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00X(H00F,H00G), C013(H01F,H01G), C01R(H01A,H01B), C02H(H02Y,
 H), C02J(H02H,H02J), C11(H11A,H11B), C14(H14A,H14B), C20B(H20A,H20B),
 C24B(H24A,H24B), C1(H1B,H1C), C5(H5A,H5B), C16(H16A,H16B), C17(H17A,H17B),
 C24A(H24C,H24D), C20A(H20C,H20D)
4.c Me refined with riding coordinates:
 C21(H21D,H21E,H21F), C21(H21A,H21B,H21C)
4.d Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C012(H012), C017(H017), C019(H019), C01A(H01H), C01C(H01I),
 C01F(H01J), C01N(H01N), C01O(H01O), C01T(H01T), C023(H023), C027(H027),
 C028(H028), C02C(H02G), C02E(H02W), C02F(H02X), C02I(H02I), C02K(H02Z),
 C02L(H02L), C02M(H02), C02R(H02R), C02S(H02S), C02X(H3), C030(H030),
 C032(H032), C036(H036), C038(H038), C03A(H03E), C03B(H03B), C03E(H03F)
4.e Idealised Me refined as rotating group:
 C00Y(H00C,H00D,H00E), C01V(H01C,H01D,H01E), C022(H02T,H02U,H02V), C025(H02A,
 H02B,H02C), C02B(H02D,H02E,H02F), C02T(H1,HA,HB), C02U(H2,HC,HD), C02V(H02K,
 H02M,H02N), C02W(H02O,H02P,H02Q), C02Y(H4,HE,HF), C02Z(H5,HG,HH), C031(H03A,
 H03C,H03D), C2(H2B,H2C,H2D), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C8(H8A,H8B,
 H8C), C10(H10A,H10B,H10C), C4(H4B,H4C,H4D), C18(H18A,H18B,H18C)
4.f Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A), O4(H4A), O3(H3B)
;
_shelx_res_checksum              60754
_olex2_submission_special_instructions 'No special instructions were received'