Multielectron redox chemistry of lanthanide Schiff-base complexes
Camp, Clément; Guidal, Valentin; Biswas, Biplab; Pécaut, Jacques; Dubois, Lionel; Mazzanti, Marinella; Chemical Science 3 (2012) 2433–; doi:10.1039/C2SC20476B

data_1556353
_publ_section_title
;
 Multielectron redox chemistry of lanthanide Schiff-base complexes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2433
_journal_paper_doi               10.1039/C2SC20476B
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C65 H53 K3 N9 O4 Tb'
_chemical_formula_weight         1300.38
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 108.494(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5693(13)
_cell_length_b                   30.262(3)
_cell_length_c                   14.6011(13)
_cell_measurement_reflns_used    3853
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2991
_cell_measurement_theta_min      3.4355
_cell_volume                     6105.1(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
1 omega 55.00 93.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 179.0000 -180.0000 38

2 omega -45.00 80.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 0.0000 -60.0000 125

3 omega 50.00 78.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 -140.0000 -108.0000 28

4 omega -26.00 11.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -18.7957 -77.0000 -90.0000 37

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.1307
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21589
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.8208
_exptl_absorpt_correction_T_min  0.5955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.590
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         10290
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.1004
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+102.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2392
_refine_ls_wR_factor_ref         0.2722
_reflns_number_gt                6348
_reflns_number_total             10290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20476b.txt
_cod_data_source_block           cc156
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556353