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_1569952
_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, 3(C12 H19 N)'
_chemical_formula_sum            'C81 H96 N3 O9 P3'
_chemical_formula_weight         1348.51
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-07-08
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.6062(4)
_cell_length_b                   26.6062(4)
_cell_length_c                   26.6062(4)
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    198.0
_cell_measurement_theta_max      61.93
_cell_measurement_theta_min      2.35
_cell_volume                     18834.3(5)
_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)'
_diffrn_ambient_temperature      198.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0673
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            137652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.699
_diffrn_reflns_theta_min         2.348
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6775
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.8996.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.951
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 2557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5819
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1861P)^2^+15.9354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.2307
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5682
_reflns_number_total             5819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           1a_sq
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_original_cell_volume        18834.3(8)
_cod_database_code               1569952
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.794(4)
 0.206(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 H00O-O004
 2.4 with sigma of 0.02
 H00N-H00Q
 2.2 with sigma of 0.02
 C00L-C00K
 1.4 with sigma of 0.0001
 C00M-C00L
 1.39 with sigma of 0.0001
 C00N-C00J
 1.36 with sigma of 0.0001
 C00V-C00X
 1.39 with sigma of 0.0001
 C00W-C00R = C6-C00R = C00T-C00Q = C00Y-C00Q
 1.56 with sigma of 0.0001
 C00J-C00O
 1.46 with sigma of 0.0001
 C00U-C00N
 1.47 with sigma of 0.0001
 C00U-C00V
 1.37 with sigma of 0.0001
4. Rigid bond restraints
 C00N, C00J, C00W, C00R
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00W, C00R, C00J, C00N
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Rotating group:
 N00B(H00N,H00O)
5.b Ternary CH refined with riding coordinates:
 C00Q(H00Q), C00R(H00R)
5.c Secondary CH2 refined with riding coordinates:
 C00I(H00D,H00F)
5.d Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00K(H00K), C00L(H00L), C00M(H00M), C00U(H00U),
 C00V(H00V), C00X(H00Z)
5.e Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00P(H00H,H00I,H00J), C00T(H00P,H00S,H00T), C00W(H00W,
 H00X,H00Y), C00Y(H00,H,HA), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8564
_shelx_fab_checksum              20265
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'