Tetraanionic biphenyl lanthanide complexes as single-molecule magnets.
Huang, Wenliang; Le Roy, Jennifer J.; Khan, Saeed I.; Ungur, Liviu; Murugesu, Muralee; Diaconescu, Paula L.; Inorganic chemistry 54 (2015) 2374–2382; doi:10.1021/ic5029788

data_4350717
_publ_section_title
;
 Tetraanionic biphenyl lanthanide complexes as single-molecule magnets.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2374
_journal_page_last               2382
_journal_paper_doi               10.1021/ic5029788
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C56 H86 Er2 Fe2 N4 Si4, 2(K C12 H24 O6), 10(C4 H8 O)'
_chemical_formula_sum            'C120 H214 Er2 Fe2 K2 N4 O22 Si4'
_chemical_formula_weight         2701.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2570(19)
_cell_length_b                   22.701(3)
_cell_length_c                   34.573(4)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      3.70
_cell_volume                     13544(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            76816
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         3.638
_diffrn_source                   'Sealed X-Ray Tube'
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             5680
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
; 
 Flack x determined using 6707 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         16722
_refine_ls_number_restraints     1143
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+6.5827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                15396
_reflns_number_total             16722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5029788_si_002.cif
_cod_data_source_block           Er2-biph-crown2
_cod_database_code               4350717
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.731
_shelxl_version_number           2013-4
_shelx_res_checksum              13699
_shelx_hkl_checksum              80755