Synthesis and Magnetochemistry of Heterometallic Triangular FeIII2LnIII (Ln = La, Gd, Tb, Dy, and Ho) and FeIII2YIII Complexes
Singh, Namrata; Das Gupta, Sayak; Butcher, Raymond J.; Christou, George; Dalton Trans.  (2017) –; doi:10.1039/C7DT00949F

data_7043244
_publ_section_title
;
 Synthesis and Magnetochemistry of Heterometallic Triangular FeIII2LnIII
 (Ln = La, Gd, Tb, Dy, and Ho) and FeIII2YIII Complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00949F
_journal_year                    2017
_chemical_formula_moiety         'C42 H54 Fe2 Gd N5 O14, C2 H3 N'
_chemical_formula_sum            'C44 H57 Fe2 Gd N6 O14'
_chemical_formula_weight         1162.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.656(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.859(3)
_cell_length_b                   19.698(5)
_cell_length_c                   20.530(5)
_cell_measurement_reflns_used    4272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.24
_cell_volume                     4780(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_number            11109
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         1.435
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.9596
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
PROBLEM: Check Calcd Residual Density  0.34A From      La       4.85 eA-3
RESPONSE: An absorption correction was applied to the data but there was still
a large peaks near the heaviest atom (Gd).
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       prism
_exptl_crystal_F_000             2364
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.523
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         11109
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+9.5371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8021
_reflns_number_total             11109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00949f2.cif
_cod_data_source_block           shelx
_cod_database_code               7043244
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41607