Epimerization effects on coordination behaviours of phenanthroline-based phosphine-oxide ligands with uranyl ions.
Yang, Xiaofan; Fang, Dong; Wang, Shihui; Tian, Zhenjiang; Xu, Lei; Liu, Jiyong; Zhang, Anyun; Xiao, Chengliang; Chemical communications (Cambridge, England) 60 (2024) 5042–5045; doi:10.1039/d4cc00258j

data_7132930
_publ_section_title
;
 Epimerization effects on coordination behaviours of phenanthroline-based
 phosphine-oxide ligands with uranyl ions.
;
_journal_issue                   38
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5042
_journal_page_last               5045
_journal_paper_doi               10.1039/d4cc00258j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C28 H26 N3 O7 P2 U), 0.5(H4 O2), 2(C3 H6 O)'
_chemical_formula_sum            'C62 H66 N6 O17 P4 U2'
_chemical_formula_weight         1767.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-31 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.0258(11)
_cell_length_b                   12.8733(5)
_cell_length_c                   16.8307(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.624
_cell_measurement_theta_min      2.842
_cell_volume                     6133.6(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5502
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.902
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_target            Mo
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    12.167
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.7445.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.308
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         5502
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+44.3724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5299
_reflns_number_total             5502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00258j2.cif
_cod_data_source_block           230220_yxf_a2
_cod_depositor_comments
'Adding full bibliography for 7132930--7132933.cif.'
_cod_database_code               7132930
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.570
_shelx_estimated_absorpt_t_min   0.338
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(2)
 0.50(2)
2. 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,H) groups
3. Restrained distances
 O11-C1G
 1.21 with sigma of 0.02
 C1G-C1H = C1G-C1I
 1.5 with sigma of 0.02
 O12-C1J
 1.21 with sigma of 0.02
 C1J-C1K = C1J-C1L
 1.5 with sigma of 0.02
 C1H-C1G = C1G-C1I
 1.52 with sigma of 0.02
 C1L-C1J = C1J-C1K
 1.52 with sigma of 0.02
 O12-C1J = O11-C1G
 1.2 with sigma of 0.005
 O11-C1H = O11-C1I
 2.38 with sigma of 0.04
 O12-C1K = O12-C1L
 2.38 with sigma of 0.04
 C1H-C1I
 2.564 with sigma of 0.04
 C1L-C1K
 2.564 with sigma of 0.04
 C1G-C1H \\sim C1G-C1I
 with sigma of 0.02
 C1H-O11 \\sim C1I-O11
 with sigma of 0.04
 C1J-C1K \\sim C1J-C1L
 with sigma of 0.02
 C1K-O12 \\sim C1L-O12
 with sigma of 0.04
4. Restrained planarity
 O11, C1G, C1H, C1I
 with sigma of 0.05
 O12, C1J, C1K, C1L
 with sigma of 0.05
5. Uiso/Uaniso restraints and constraints
O11 \\sim C1G \\sim C1H \\sim C1I: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C1G \\sim O11 \\sim C1H \\sim C1I: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
O12 \\sim C1J \\sim C1K \\sim C1L: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6. Rigid body (RIGU) restrains
 O11, C1G, C1H, C1I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, C1J, C1K, C1L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O12)=Sof(C1J)=Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=Sof(C1L)=Sof(H1LA)=
 Sof(H1LB)=Sof(H1LC)=1-FVAR(1)
 Sof(O11)=Sof(C1G)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=Sof(C1I)=Sof(H1IA)=
 Sof(H1IB)=Sof(H1IC)=FVAR(1)
 Fixed Sof: H9A(0.5) H9B(0.5)
8.a Everything fixed:
 O9, H9A, H9B
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
8.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
8.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C22(H22A,H22B,H22C), C1H(H1HA,H1HB,H1HC), C1I(H1IA,H1IB,
 H1IC), C1K(H1KA,H1KB,H1KC), C1L(H1LA,H1LB,H1LC)
;
_shelx_res_checksum              42159
_shelx_hkl_checksum              78075
_olex2_submission_special_instructions 'No special instructions were received'