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_1569963
_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_absolute_configuration ad
_chemical_formula_moiety         'C45 H39 O9 P3, C8 H8 O'
_chemical_formula_sum            'C53 H47 O10 P3'
_chemical_formula_weight         936.81
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2023-01-07
_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                75.792(2)
_cell_angle_beta                 87.279(2)
_cell_angle_gamma                77.210(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3298(3)
_cell_length_b                   11.7921(6)
_cell_length_c                   23.5575(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      27.530
_cell_measurement_theta_min      2.216
_cell_volume                     2187.46(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55174
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.783
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.9537.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       needle
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 5870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         19034
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0583P)^2^+0.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                15088
_reflns_number_total             19034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           1a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569963
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.942
_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.a Ternary CH refined with riding coordinates:
 C037(H037), C03M(H03N)
2.b Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C01A(H01A,H01B), C01B(H01C,H01D), C01E(H01S,H01T), C01R(H01U,
 H01V), C02H(H02W,H02X), C03E(H03J,H03L), C03J(H03P,H03Q)
2.c Aromatic/amide H refined with riding coordinates:
 C012(H012), C014(H014), C016(H016), C01D(H01E), C01H(H01H), C01M(H01M),
 C01N(H01N), C01O(H01O), C022(H022), C026(H026), C027(H027), C029(H029),
 C02C(H02C), C02I(H02Z), C02J(H02), C02K(H5), C02M(H1), C02Q(H2), C02R(H3),
 C02T(H4), C02U(H6), C02W(H7), C02Y(H02Y), C030(H030), C032(H032), C033(H033),
 C034(H034), C035(H035), C038(H038), C039(H039), C03B(H03D), C03C(H03E),
 C03D(H03F), C03G(H03G), C03H(H03H), C03I(H03I), C03K(H03K), C03L(H03M),
 C03N(H03R), C03O(H03O)
2.d Idealised Me refined as rotating group:
 C019(H01J,H01K,H01L), C01C(H01P,H01Q,H01R), C01U(H01W,H01X,H01Y), C01W(H01F,
 H01G,H01I), C020(H02N,H02O,H02P), C021(H02Q,H02R,H02S), C02F(H02T,H02U,H02V),
 C02P(H02A,H02B,H02D), C02S(H02E,H02F,H02G), C02X(H02H,H02I,H02J), C02Z(H02K,
 H02L,H02M), C031(H03A,H03B,H03C)
;
_shelx_res_checksum              16263
_olex2_submission_special_instructions 'No special instructions were received'