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_1556351
_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            'C108.1 H150.89 K N4 Nd O12'
_chemical_formula_weight         1881.70
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                90.671(6)
_cell_angle_beta                 113.704(7)
_cell_angle_gamma                96.867(6)
_cell_formula_units_Z            2
_cell_length_a                   16.1709(13)
_cell_length_b                   17.5403(13)
_cell_length_c                   19.5362(15)
_cell_measurement_reflns_used    3209
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9683
_cell_measurement_theta_min      3.3687
_cell_volume                     5026.5(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SUPERFLIP
Palatinus, L. & Chapuis, G. (2007). SUPERFLIP - a computer program for the solution of crystal structures by charge flipping in arbitrary dimensions, J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
1 omega -49.00 43.00 1.0000 80.0000
omega____ theta____ kappa____ phi______ frames
- 17.1550 -37.0000 120.0000 92

2 omega -23.00 60.00 1.0000 80.0000
omega____ theta____ kappa____ phi______ frames
- 17.1550 -101.0000 80.0000 83

3 omega -9.00 90.00 1.0000 80.0000
omega____ theta____ kappa____ phi______ frames
- 17.1550 37.0000 -60.0000 99

4 omega -25.00 23.00 1.0000 80.0000
omega____ theta____ kappa____ phi______ frames
- -18.8738 -99.0000 -60.0000 48

5 omega -92.00 -2.00 1.0000 80.0000
omega____ theta____ kappa____ phi______ frames
- -18.8738 -19.0000 30.0000 90

;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2504
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28488
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.7391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             2005
_exptl_crystal_size_max          0.5203
_exptl_crystal_size_mid          0.1550
_exptl_crystal_size_min          0.0354
_refine_diff_density_max         2.407
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         28488
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                14757
_reflns_number_total             28488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20476b.txt
_cod_data_source_block           vg47-2_hklf5
_cod_original_formula_sum        'C108.10 H150.89 K N4 Nd O12'
_cod_database_code               1556351
_cell_oxdiff_twin_number         2