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_1569960
_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, 2(C9 H14 O)'
_chemical_formula_sum            'C63 H67 O11 P3'
_chemical_formula_weight         1093.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2023-01-08
_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                116.041(3)
_cell_angle_beta                 91.906(3)
_cell_angle_gamma                102.985(3)
_cell_formula_units_Z            4
_cell_length_a                   17.9616(9)
_cell_length_b                   18.1401(10)
_cell_length_c                   19.7987(11)
_cell_measurement_reflns_used    9236
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      68.34
_cell_measurement_theta_min      3.26
_cell_volume                     5583.3(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.988
_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  0.0732
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73795
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.717
_diffrn_reflns_theta_min         2.512
_diffrn_source_current           1.11
_diffrn_source_power             0.0555
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1484 before and 0.0753 after correction.
The Ratio of minimum to maximum transmission is 0.7347.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1525
_refine_ls_number_reflns         20406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1077P)^2^+3.6113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16295
_reflns_number_total             20406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02995f2.cif
_cod_data_source_block           cu_jjm_347_0m
_cod_depositor_comments
'Adding full bibliography for 1569950--1569976.cif.'
_cod_original_cell_volume        5583.3(5)
_cod_database_code               1569960
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.842
_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. Others
 Sof(H03Q)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C26)=
 Sof(O27)=1-FVAR(1)
 Sof(H03P)=Sof(C03J)=Sof(H03R)=Sof(H03S)=Sof(O03T)=Sof(C041)=Sof(C047)=
 Sof(H04I)=Sof(H04J)=Sof(C048)=Sof(H04K)=Sof(H04L)=Sof(H04M)=Sof(C04A)=
 Sof(H04N)=Sof(H04O)=Sof(H04P)=FVAR(1)
 Sof(HJ)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O15)=Sof(C6)=1-FVAR(2)
 Sof(O02W)=Sof(H12)=Sof(C03V)=Sof(C03Y)=Sof(H03G)=Sof(H03J)=Sof(C042)=
 Sof(H04A)=Sof(H04B)=Sof(H04C)=Sof(C044)=Sof(H04D)=Sof(H04E)=Sof(C049)=
 Sof(H04F)=Sof(H04G)=Sof(H04H)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C00Q(H00A,H00B), C010(H01A,H01B), C013(H01E,H01F), C015(H01G,H01H), C017(H01I,
 H01J), C01M(H01C,H01D), C034(H03T,H03U), C03J(H03R,H03S), C03M(H03Y,HK),
 C03X(H15,HN), C03Y(H03G,H03J), C040(H04Q,H04R), C044(H04D,H04E), C047(H04I,
 H04J), C4(H4A,H4B), C22(H22A,H22B), C5(H5A,H5B), C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C020(H020), C021(H021), C022(H022), C024(H024), C025(H025), C028(H028),
 C02C(H02D), C02F(H1), C02J(H02T), C02M(H02U), C02N(H4), C02O(H5), C02Q(H6),
 C02R(H7), C02T(H9), C02V(H02V), C02X(H12), C02X(HJ), C02Y(H11), C02Z(H02Z),
 C030(H030), C033(H033), C036(H036), C037(H037), C039(H039), C03C(H03P),
 C03C(H03Q), C03D(H03D), C03E(H03E), C03F(H03F), C03H(H03H), C03I(H03I),
 C03K(H03K), C03L(H03L), C03S(H03Z), C03U(H14)
3.c Idealised Me refined as rotating group:
 C029(H02W,H02X,H02Y), C02A(H02,H,HA), C02B(H02A,H02B,H02C), C02D(H02E,H02F,
 H02G), C02E(H02H,H02I,H02J), C02G(H02K,H02L,H02M), C02H(H02N,H02O,H02P),
 C02I(H02Q,H02R,H02S), C02K(H2,HB,HC), C02L(H3,HD,HE), C02S(H8,HF,HG), C02U(H10,
 HH,HI), C032(H03M,H03N,H03O), C03A(H03A,H03B,H03C), C03G(H03V,H03W,H03X),
 C03W(H03,HL,HM), C03Z(H13,HO,HP), C042(H04A,H04B,H04C), C043(H04S,H04T,H04U),
 C045(H04V,H04W,H04X), C046(H04Y,HQ,HR), C048(H04K,H04L,H04M), C049(H04F,H04G,
 H04H), C04A(H04N,H04O,H04P), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C),
  C3(H3A,H3B,H3C)
;
_shelx_res_checksum              70081
_olex2_submission_special_instructions 'No special instructions were received'