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_1556354
_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            'C64 H78 I K2 N4 Nd O16'
_chemical_formula_weight         1508.64
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/n 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                 89.466(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.0578(5)
_cell_length_b                   12.1559(4)
_cell_length_c                   19.0780(7)
_cell_measurement_reflns_used    3310
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4098
_cell_measurement_theta_min      3.4971
_cell_volume                     3260.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
1 omega 60.00 92.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 179.0000 -150.0000 32

2 omega -79.00 24.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 0.0000 -90.0000 103

3 omega 3.00 46.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 45.0000 114.0000 43

4 omega 61.00 93.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 30.0000 32

5 omega -88.00 -58.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 131.0000 -13.0000 30

;
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15573
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.8768
_exptl_absorpt_correction_T_min  0.3306
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.97
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.314
_refine_diff_density_min         -4.005
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0854P)^2^+20.3814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                6051
_reflns_number_total             8058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20476b.txt
_cod_data_source_block           bi250
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               1556354