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_7038443
_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 La N3 O15 P4, 2.33(C2 H3 N)'
_chemical_formula_sum            'C60.67 H59 La N5.33 O15 P4'
_chemical_formula_weight         1365.59
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_audit_update_record
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.709(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.444(8)
_cell_length_b                   17.849(9)
_cell_length_c                   26.571(15)
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    120
_cell_measurement_theta_max      22.95
_cell_measurement_theta_min      2.41
_cell_volume                     6376(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2178
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8845
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.69
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)''
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2789
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.207
_refine_diff_density_min         -4.243
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00155(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+110.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2451
_reflns_number_gt                4827
_reflns_number_total             8846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04963f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7038440--7038445.cif.'
_cod_original_cell_volume        6375(6)
_cod_database_code               7038443
_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
 C4S-C3S
 1.5 with sigma of 0.02
 C4S-N2S
 1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C8) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(N2S) = Uanis(C4S) = Uanis(C3S)
4. Others
 Fixed Sof: C3S(0.16667) H3SA(0.16667) H3SB(0.16667) H3SC(0.16667)
 N2S(0.16667) C4S(0.16667)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
5.d 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)
;
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'