Di-maltol-polyamine ligands to form heterotrinuclear metal complexes: solid state, aqueous solution and magnetic characterization.
Benelli, Cristiano; Borgogelli, Elisa; Formica, Mauro; Fusi, Vieri; Giorgi, Luca; Macedi, Eleonora; Micheloni, Mauro; Paoli, Paola; Rossi, Patrizia; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5848–5859; doi:10.1039/c3dt32130d

data_7022601
_publ_section_title
;
 Di-maltol-polyamine ligands to form heterotrinuclear metal complexes:
 solid state, aqueous solution and magnetic characterization.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5848
_journal_page_last               5859
_journal_paper_doi               10.1039/c3dt32130d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C44 H64 Cl3 Co2 Gd N8 O26'
_chemical_formula_weight         1502.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.196(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4681(5)
_cell_length_b                   24.7525(7)
_cell_length_c                   15.9297(5)
_cell_measurement_reflns_used    11336
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.5319
_cell_measurement_theta_min      3.7336
_cell_volume                     5606.0(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42128
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedal
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         18089
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                8902
_reflns_number_total             18089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32130d.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7022601
_vfr_plat_973
;
PROBLEM: Large calc. positive residual density on Gd1
RESPONSE: The high max. difference electron density peak of 1.453
is located at a distance of 0.95 A from Gd1.
;
_vfr_plat_420
;
PROBLEM: D-H without acceptor ...O1W-H1WB
RESPONSE: A weak hydrogen bond (according to G. R. Desiraju and T. Steiner,
The Weak Hydrogen Bond, Oxford University Press, 2001) involving the
hydrogen atom H1WB and the symmetry related oxygen atom O23'
(' = -x, y+0.5, -z+1.5) is present. The H1WB...O23' distance is 3.0(1)A)
;
_vfr_plat_910
;
PROBLEM: Missing # of FCF Reflections Below Th(Min) ..... 37
RESPONSE:
Data were collected with a CCD detector. The reflections in question were
affected by the beam-stop. Only a small number of reflections are missing
out of the total number of reflections observed.
Resolution and completeness statistics
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
Theta sin(th)/Lambda Complete Expected Measured Missing
20.82 0.500 0.994 5875 5837 38
23.01 0.550 0.995 7803 7763 40
25.24 0.600 0.995 10144 10096 48
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