Preparation of n,n-dialkylcarbamato lanthanide complexes by extraction of lanthanide ions from aqueous solution into hydrocarbons.
Armelao, Lidia; Belli Dell'Amico, Daniela; Biagini, Paolo; Bottaro, Gregorio; Chiaberge, Stefano; Falvo, Paola; Labella, Luca; Marchetti, Fabio; Samaritani, Simona; Inorganic chemistry 53 (2014) 4861–4871; doi:10.1021/ic402936z

data_4338269
_publ_section_title
;
 Preparation of n,n-dialkylcarbamato lanthanide complexes by extraction of
 lanthanide ions from aqueous solution into hydrocarbons.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4861
_journal_page_last               4871
_journal_paper_doi               10.1021/ic402936z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C109 H216 N12 O27 Tb4, 2(C8 H20 N)'
_chemical_formula_sum            'C125 H256 N14 O27 Tb4'
_chemical_formula_weight         3023.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.963(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.399(6)
_cell_length_b                   27.759(5)
_cell_length_c                   17.295(3)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.36
_cell_volume                     15054(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_sigmaI/netI    0.1391
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            141804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.2100
_exptl_absorpt_correction_T_min  0.1338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2008-1'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Splinter
_exptl_crystal_F_000             6320
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         5.364
_refine_diff_density_min         -4.680
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1527
_refine_ls_number_reflns         36027
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.2179
_refine_ls_R_factor_gt           0.1186
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+724.7388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2909
_refine_ls_wR_factor_ref         0.3472
_reflns_number_gt                19889
_reflns_number_total             36027
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic402936z_si_001.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338269.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4338269