Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen2−)
Barbosa, Guilherme Augusto; Santana, Francielli Sousa; Nunes, Giovana Gioppo; Soares, Jaísa Fernandes; Acta Crystallographica Section E Crystallographic Communications 75 (2019) 418–; doi:10.1107/S2056989019002998

data_2021536
_publ_section_title
;
 Crystal structures of binuclear complexes of gadolinium(III) and
 dysprosium(III) with oxalate bridges and chelating
 N,N&#x2032;-bis(2-oxidobenzyl)-N,N&#x2032;-bis(pyridin-2-ylmethyl)ethylenediamine
 (bbpen2&#x2212;)
;
_journal_coeditor_code           WM5489
_journal_issue                   4
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              418
_journal_paper_doi               10.1107/S2056989019002998
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Gd2 (C28 H28 N4 O2)2 (C2 O4)], 4C H4 O, 4H2 O'
_chemical_formula_moiety         'C58 H56 Gd2 O8 N8, 4(C H4 O), 4(H2 O)'
_chemical_formula_structural     '[Gd2C58H56O8N8].4(CH3OH).4(H2O)'
_chemical_formula_sum            'C62 H80 Gd2 N8 O16'
_chemical_formula_weight         1507.84
_chemical_name_systematic
'(\m-Oxalato)bis{[<i>N</i>,<i>N</i>'-bis(2-oxidobenzyl-\k<i>O</i>)-<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl-\k<i>N</i>)ethylenediamine-\k^2^<i>N</i>,<i>N</i>']gadolinium(III)}--methanol--water (1/4/4)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                69.092(4)
_cell_angle_beta                 74.786(4)
_cell_angle_gamma                70.324(4)
_cell_formula_units_Z            1
_cell_length_a                   9.8778(11)
_cell_length_b                   12.8720(16)
_cell_length_c                   14.8025(18)
_cell_measurement_reflns_used    9519
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.98
_cell_volume                     1633.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
ORTEP (Johnson, 1976 and Farrugia, 2012) and DIAMOND
(Brandenburg, 2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and WINGX (Farrugia, 1999,
2012)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i>  (Sheldrick 2015b)
;
_computing_structure_solution
;
SHELXT2015 (Sheldrick 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            101878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.145
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.548
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7108
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0132P)^2^+1.5506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                6476
_reflns_number_total             7108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5489sup1.cif
_cod_data_source_block           1
_cod_database_code               2021536
_shelx_estimated_absorpt_t_min   0.572
_shelx_estimated_absorpt_t_max   0.752
_shelx_hkl_checksum              36044
_shelx_res_checksum              22281
_shelx_fab_checksum              42849
_cod_database_fobs_code 2021536