Synthesis of novel lanthanide acylpyrazolonato ligands with long aliphatic chains and immobilization of the Tb complex on the surface of silica pre-modified via hydrophobic interactions.
Pettinari, C.; Marchetti, F.; Pettinari, R.; Belousov, Y. A.; Taydakov, I. V.; Krasnobrov, V. D.; Petukhov, D. I.; Drozdov, A. A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14887–14895; doi:10.1039/c5dt01964h

data_7035808
_publ_section_title
;
 Synthesis of novel lanthanide acylpyrazolonato ligands with long
 aliphatic chains and immobilization of the Tb complex on the surface of
 silica pre-modified via hydrophobic interactions.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14887
_journal_page_last               14895
_journal_paper_doi               10.1039/c5dt01964h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C84 H133 N6 O8 Y'
_chemical_formula_sum            'C84 H133 N6 O8 Y'
_chemical_formula_weight         1443.87
_chemical_properties_physical    Heat-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-25 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                84.792(3)
_cell_angle_beta                 74.088(3)
_cell_angle_gamma                65.143(3)
_cell_formula_units_Z            2
_cell_length_a                   15.101(3)
_cell_length_b                   15.292(3)
_cell_length_c                   20.498(4)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.90
_cell_measurement_theta_min      2.33
_cell_volume                     4128.8(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20397
_diffrn_reflns_theta_full        20.20
_diffrn_reflns_theta_max         20.20
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1564
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         7907
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+7.6818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                5600
_reflns_number_total             7907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01964h2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 7035808.cif.'
_cod_original_cell_volume        4129.0(14)
_cod_database_code               7035808