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_1569971
_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, 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             2022-06-29
_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                 116.4770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5584(4)
_cell_length_b                   10.1939(2)
_cell_length_c                   24.3804(4)
_cell_measurement_reflns_used    9123
_cell_measurement_temperature    198.0
_cell_measurement_theta_max      67.92
_cell_measurement_theta_min      4.05
_cell_volume                     5018.43(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 0.970
_diffrn_measured_fraction_theta_max 0.966
_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  0.1191
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            184212
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.154
_diffrn_reflns_theta_min         2.024
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 6774 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         16911
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0707P)^2^+1.8385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    0.879
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                15969
_reflns_number_total             16911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           1a_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_original_cell_volume        5018.42(16)
_cod_database_code               1569971
_shelx_shelxl_version_number     2014/7
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C02J(H4), C03F(H9), C03H(H03), C03O(H03V)
2.b Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00T(H00C,H00D), C011(H01N,H01P), C017(H01A,H01B), C01A(H01R,
 H01S), C02N(H5,H), C02S(H02Z,HC), C03D(H03Z,HH), C03I(H03J,H03K), C03M(H03R,
 H03S), C03N(H03T,H03U), C03P(H10,HK), C03R(H11,HL), C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00W(H00W), C014(H014), C01B(H01C), C01I(H01T), C01L(H01L),
 C01O(H01O), C01Q(H01Q), C01V(H01V), C025(H025), C026(H026), C027(H027),
 C029(H029), C02B(H02N), C02L(H02L), C02M(H02V), C02P(H02P), C02Q(H02X),
 C02V(H02), C02W(H02W), C02X(H1), C02Y(H2), C030(H030), C031(H031), C035(H035),
 C038(H038), C039(H039), C03A(H03D), C03C(H03E), C03G(H03G)
2.d Tetrahedral OH refined with riding coordinates:
 O010(H010)
2.e Idealised Me refined as rotating group:
 C01G(H01D,H01E,H01F), C01P(H01G,H01H,H01I), C01X(H01J,H01K,H01M), C021(H02A,
 H02B,H02C), C028(H02J,H02K,H02M), C02A(H02D,H02E,H02F), C02E(H02O,H02Q,H02R),
 C02G(H02S,H02T,H02U), C02R(H02Y,HA,HB), C02T(H02G,H02H,H02I), C02Z(H3,HD,HE),
 C032(H8,HF,HG), C034(H03A,H03B,H03C), C03E(H03F,H03H,H03I), C03J(H7,HI,HJ),
 C03K(H03L,H03M,H03N), C03L(H03O,H03P,H03Q), C03Q(H03W,H03X,H03Y), C2(H2A,H2B,
 H2C), C3(H3A,H3B,H3C)
2.f Idealised tetrahedral OH refined as rotating group:
 O00M(H00M), O02H(H6), O033(H033)
;
_shelx_res_checksum              76848
_olex2_submission_special_instructions 'No special instructions were received'