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_7132933
_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         'C28 H26 N2 O2 P2'
_chemical_formula_sum            'C28 H26 N2 O2 P2'
_chemical_formula_weight         484.45
_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             2023-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                73.8290(10)
_cell_angle_beta                 85.3630(10)
_cell_angle_gamma                76.8650(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2310(3)
_cell_length_b                   11.7984(5)
_cell_length_c                   13.6524(5)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.552
_cell_measurement_theta_min      2.540
_cell_volume                     1239.83(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62474
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.065
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9678.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0409P)^2^+0.5469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5400
_reflns_number_total             5697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00258j2.cif
_cod_data_source_block           230905_et_ph_rr
_cod_depositor_comments
'Adding full bibliography for 7132930--7132933.cif.'
_cod_database_code               7132933
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.919
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              36803
_shelx_hkl_checksum              82557
_olex2_submission_special_instructions 'No special instructions were received'