pH-dependent phosphate separation using tripodal hexaurea receptor
Sun, Zhong-Yu; Chen, Si-Qi; Liang, Lin; Zhao, Wei; Yang, Xiao-Juan; Wu, Biao; Chemical Communications  (2023) –; doi:10.1039/D3CC04122K

data_7132159
_publ_section_title
;
 pH-dependent phosphate separation using tripodal hexaurea receptor
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04122K
_journal_year                    2023
_chemical_formula_moiety
'O4 P, C48 H48 N16 O12, 3(C4 H12 N), 2(C2 H3 N)'
_chemical_formula_sum            'C64 H90 N21 O16 P'
_chemical_formula_weight         1440.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-28 deposited with the CCDC.	2023-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9758(14)
_cell_length_b                   23.4980(15)
_cell_length_c                   14.4237(9)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      2.24
_cell_volume                     7448.2(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            100465
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.150
_diffrn_reflns_theta_max         25.150
_diffrn_reflns_theta_min         2.236
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1281 before and 0.0842 after correction.
The Ratio of minimum to maximum transmission is 0.9024.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6725
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 3753 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.0064(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         13296
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0537P)^2^+7.4233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                10233
_reflns_number_total             13296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04122k2.cif
_cod_data_source_block           02_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7132159
_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. Restrained distances
 N22-C66
 2.6 with sigma of 0.02
 O12-N16 = O11-N16
 1.21 with sigma of 0.02
 C59-C60 = C57-C58 = C57-C59 = C57-C60 = C58-C59
 2.5 with sigma of 0.02
 N19-C57 = N19-C58 = N19-C59 = N19-C60
 1.5 with sigma of 0.02
 N21-C63 = N22-C65 = N23-C67 = N24-C69
 1.14 with sigma of 0.02
 C63-C64 = C65-C66 = C67-C68 = C69-C70
 1.46 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N19 \\sim C57 \\sim C58 \\sim C60 \\sim N22 \\sim C65 \\sim C66 \\sim N23 \\sim
C67 \\sim C68: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(N19) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(N21)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(N22) \\sim Ueq,
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: N19(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) H59C(0.5) C65(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) N22(0.5)
 C63(0.6) N21(0.6) C64(0.6) H64A(0.6) H64B(0.6) H64C(0.6) C70(0.4) H70A(0.4)
 H70B(0.4) H70C(0.4) C69(0.4) N24(0.4) C67(0.5) C68(0.5) H68A(0.5) H68B(0.5)
 H68C(0.5) N23(0.5)
5.a Riding coordinates:
 C57(H57A,H57B,H57C)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C34(H34A,H34B), C33(H33A,H33B), C1(H1A,H1B),
 C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 N14(H14), N13(H13), N8(H8), N7(H7), N15(H15), N5(H5), N9(H9), N12(H12),
 N4(H4), N2(H2), N3(H3), N10(H10), C16(H16), C13(H13A), C15(H15A), C37(H37),
 C40(H40), C12(H12A), C31(H31), C32(H32), C24(H24), C44(H44), C45(H45),
 C21(H21), C48(H48), C39(H39), C38(H38), C8(H8A), C47(H47), C0AA(H0AA),
 C22(H22), C7(H7A), C5(H5A), C6(H6), C28(H28), C29(H29)
5.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C49(H49A,H49B,H49C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C), C60(H60A,H60B,H60C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C66(H66A,H66B,H66C), C64(H64A,H64B,
 H64C), C70(H70A,H70B,H70C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              51129
_shelx_hkl_checksum              48848
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'