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_1569968
_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, C6 H9 N O3'
_chemical_formula_sum            'C51 H48 N O12 P3'
_chemical_formula_weight         959.81
_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             2022-11-28
_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                62.242(2)
_cell_angle_beta                 89.152(2)
_cell_angle_gamma                84.690(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6588(5)
_cell_length_b                   16.0406(8)
_cell_length_c                   16.4140(8)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.04
_cell_volume                     2239.6(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.998
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            84720
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.336
_diffrn_reflns_theta_min         3.044
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.793
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1491 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.8533.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 6772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         15926
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0804P)^2^+0.7004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                14826
_reflns_number_total             15926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           q1_CCDC7
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_database_code               1569968
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C03M) \\sim Ueq, Uanis(C03I) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.012
3.a Ternary CH refined with riding coordinates:
 C039(H039), C2(H2A)
3.b Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B), C010(H01C,H01D), C01B(H01A,H01B), C025(H02S,H02T), C02D(H02I,
 H02J), C02I(H02L,H02M), C03C(H03S,H03T), C03I(H03O,H03P), C03M(H03Q,H03R),
 C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00Z(H00Z), N01A(H01L), C01C(H01F), C01E(H01E), C01J(H01J),
 C01K(H01K), C01Q(H01Q), C01U(H01U), C01W(H01W), C01Z(H01Z), C02B(H02G),
 C02C(H02H), C02F(H02K), C02H(H02), C02K(H02N), C02L(H02O), C02N(H1), C02O(H2),
 C02P(H3), C02R(H5), C02S(H6), C02U(H7), C032(H032), C034(H034), C036(H036),
 C038(H038), C03A(H03G), C03B(H03H), C03D(H03L), N03G(H03N), C03J(H03M)
3.d Idealised Me refined as rotating group:
 C00W(H00C,H00D,H00E), C01P(H01G,H01H,H01I), C021(H02A,H02B,H02C), C023(H02D,
 H02E,H02F), C027(H02U,H02V,H02W), C028(H02X,H02Y,H), C029(H8,HA,HB), C02A(H02Z,
 HC,HD), C02Q(H4,HE,HF), C02T(H02P,H02Q,H02R), C033(H03A,H03B,H03C), C037(H03D,
 H03E,H03F), C03K(H03I,H03J,H03K), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              15287
_olex2_submission_special_instructions 'No special instructions were received'