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_7038444
_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 N3 Nd O15 P4, 3(C2 H3 N)'
_chemical_formula_sum            'C62 H61 N6 Nd O15 P4'
_chemical_formula_weight         1398.28
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-19
_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
_cell_angle_beta                 91.3780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4706(8)
_cell_length_b                   17.8919(10)
_cell_length_c                   26.4711(15)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.62
_cell_measurement_theta_min      2.40
_cell_volume                     6378.1(6)
_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      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            44834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.673
_diffrn_reflns_theta_min         1.539
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.3380
_exptl_absorpt_correction_T_min  0.2324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0381 after correction.
The Ratio of minimum to maximum transmission is 0.6876.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       needle
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         10755
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+5.7460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10078
_reflns_number_total             10755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04963f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7038440--7038445.cif.'
_cod_database_code               7038444
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.763
_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. Restrained distances
 N2S-C3S
 1.1 with sigma of 0.005
 C3S-C4S
 1.5 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(N2S) = Uanis(C3S) = Uanis(C4S)
4. Others
 Fixed Sof: C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C3S(0.5) N2S(0.5)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA)
5.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              28138