Tetranuclear Lanthanide(III) Complexes with a Zigzag Topology from the Use of Pyridine-2,6-dimethanol: Synthetic, Structural, Spectroscopic, Magnetic and Photoluminescence Studies.
Alexandropoulos, Dimitris I.; Cunha-Silva, Luís; Pham, Linh; Bekiari, Vlasoula; Christou, George; Stamatatos, Theocharis C.; Inorganic chemistry 53 (2014) 3220–3229; doi:10.1021/ic5001045

data_4337649
_publ_section_title
;
 Tetranuclear Lanthanide(III) Complexes with a Zigzag Topology from the
 Use of Pyridine-2,6-dimethanol: Synthetic, Structural, Spectroscopic,
 Magnetic and Photoluminescence Studies.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3220
_journal_page_last               3229
_journal_paper_doi               10.1021/ic5001045
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C56 H66 N10 O22 Tb4, 4(N O3), 2(C H4 O)'
_chemical_formula_sum            'C58 H74 N14 O36 Tb4'
_chemical_formula_weight         2178.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '04 December 2013'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.407(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2655(18)
_cell_length_b                   14.9732(16)
_cell_length_c                   16.0103(19)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.55
_cell_volume                     3656.3(7)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_molecular_graphics    'SHELXTL '
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXTL '
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            150416
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.5550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.309
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9057
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0070P)^2^+24.9771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                8319
_reflns_number_total             9057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5001045_si_002.cif
_cod_data_source_block           comp3-Tb-da457
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4337649