Extraction and coordination studies of a carbonyl-phosphine oxide scorpionate ligand with uranyl and lanthanide(iii) nitrates: structural, spectroscopic and DFT characterization of the complexes.
Matveeva, Anna G.; Vologzhanina, Anna V.; Goryunov, Evgenii I.; Aysin, Rinat R.; Pasechnik, Margarita P.; Matveev, Sergey V.; Godovikov, Ivan A.; Safiulina, Alfiya M.; Brel, Valery K.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5162–5179; doi:10.1039/c5dt04963f

data_7038445
_publ_section_title
;
 Extraction and coordination studies of a carbonyl-phosphine oxide
 scorpionate ligand with uranyl and lanthanide(iii) nitrates: structural,
 spectroscopic and DFT characterization of the complexes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5162
_journal_page_last               5179
_journal_paper_doi               10.1039/c5dt04963f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C56 H52 N2 Nd O12 P4, N O3, C2 H6 O'
_chemical_formula_sum            'C58 H58 N3 Nd O16 P4'
_chemical_formula_weight         1321.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.574(16)
_cell_angle_beta                 96.836(16)
_cell_angle_gamma                111.923(17)
_cell_formula_units_Z            2
_cell_length_a                   12.590(7)
_cell_length_b                   13.510(10)
_cell_length_c                   19.148(15)
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    120
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.25
_cell_volume                     2995(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1446
_diffrn_reflns_av_unetI/netI     0.2429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38088
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.906
_diffrn_reflns_theta_min         1.628
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.493
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       prism
_exptl_crystal_F_000             1350
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.962
_refine_diff_density_min         -2.742
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         17037
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1646
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8453
_reflns_number_total             17037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04963f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7038440--7038445.cif.'
_cod_original_cell_volume        2994(4)
_cod_database_code               7038445
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.795
_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, All O(H) groups
2. Restrained distances
 C2S-C1S
 1.5 with sigma of 0.02
 O1S-C1S
 1.4 with sigma of 0.02
 C3S-C4S
 1.5 with sigma of 0.02
 O2S-C3S
 1.4 with sigma of 0.02
 C2S-C1S
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C4S)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O1S) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(O1S) = Uanis(O2S)
Uanis(C3S) = Uanis(C1S)
Uanis(C2S) = Uanis(C4S)
4. Others
 Fixed Sof: O1S(0.5) H1A(0.5) O2S(0.5) H10(0.5) C1S(0.5) H2A(0.5) H2B(0.5)
 C2S(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C4S(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C3S(0.5) H15A(0.5) H15B(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C30(H30A,H30B), C1S(H2A,H2B), C3S(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10D), C12(H12), C13(H13), C14(H14),
 C1AA(H1AA), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56)
5.d Tetrahedral OH refined with riding coordinates:
 O1S(H1A), O2S(H10)
5.e Idealised Me refined as rotating group:
 C4(H4D,H4E,H4F), C32(H32A,H32B,H32C), C2S(H4A,H4B,H4C), C4S(H10A,H10B,H10C)
;
_shelx_res_checksum              28552