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_1556352
_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            'C177.5 H141.5 K9 N23.5 Nd3 O12'
_chemical_formula_weight         3580.26
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 97.395(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.6191(5)
_cell_length_b                   27.7932(8)
_cell_length_c                   19.0450(6)
_cell_measurement_reflns_used    20802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5042
_cell_measurement_theta_min      3.3043
_cell_volume                     8198.8(4)
_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
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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
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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      293(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -25.00 74.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 0.0000 -120.0000 99

2 omega -104.00 -58.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 179.0000 -120.0000 46

3 omega -76.00 3.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 -77.0000 -120.0000 79

4 omega 65.00 101.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 -30.0000 36

5 omega 57.00 94.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 150.0000 37

6 omega -47.00 26.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 -37.0000 -120.0000 73

7 omega -52.00 40.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.2801 37.0000 -180.0000 92

8 omega -75.00 -48.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.2801 110.0000 -49.0000 27

;
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.1004
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83596
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.8206
_exptl_absorpt_correction_T_min  0.7280
_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            black
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3636
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.026
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.463(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2014
_refine_ls_number_reflns         40613
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+10.1541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                31026
_reflns_number_total             40613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20476b.txt
_cod_data_source_block           cc180
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C177.50 H141.50 K9 N23.50 Nd3 O12'
_cod_database_code               1556352