Seven-coordinate lanthanide complexes with a tripodal redox active ligand: structural, electrochemical and spectroscopic investigations.
Molloy, Jennifer K.; Philouze, Christian; Fedele, Lionel; Imbert, Daniel; Jarjayes, Olivier; Thomas, Fabrice; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10742–10751; doi:10.1039/c8dt01165f

data_7046778
_publ_section_title
;
 Seven-coordinate lanthanide complexes with a tripodal redox active
 ligand: structural, electrochemical and spectroscopic investigations.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10742
_journal_page_last               10751
_journal_paper_doi               10.1039/c8dt01165f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C42 H57 N4 Nd1 O6, 2(H2 O)'
_chemical_formula_sum            'C42 H61 N4 Nd O8'
_chemical_formula_weight         894.18
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.881(2)
_cell_length_b                   15.881(2)
_cell_length_c                   10.323(2)
_cell_measurement_reflns_used    23017
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.067
_cell_measurement_theta_min      2.962
_cell_volume                     2254.7(6)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23017
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.067
_diffrn_reflns_theta_min         2.962
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.651588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1220 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.6516.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1937 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_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     179
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.6234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4095
_reflns_number_total             4351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01165f2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7046778--7046783.cif.'
_cod_original_cell_volume        2254.7(8)
_cod_database_code               7046778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              12044
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'