A new synthetic route towards binuclear 3d–4f complexes, using non-compartmental ligands derived from o-vanillin. Syntheses, crystal structures, magnetic and luminescent properties
Sarwar, Masood; Madalan, Augustin M.; Tiseanu, Carmen; Novitchi, Ghenadie; Maxim, Catalin; Marinescu, Gabriela; Luneau, Dominique; Andruh, Marius; New Journal of Chemistry 37 (2013) 2280–; doi:10.1039/c3nj00199g

data_7053062
_publ_section_title
;
 A new synthetic route towards binuclear 3d--4f complexes, using
 non-compartmental ligands derived from o-vanillin. Syntheses, crystal
 structures, magnetic and luminescent properties
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2280
_journal_paper_doi               10.1039/c3nj00199g
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C32 H33 Cu Gd N8 O13'
_chemical_formula_weight         958.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 104.879(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8607(6)
_cell_length_b                   11.2122(4)
_cell_length_c                   20.4234(7)
_cell_measurement_reflns_used    50377
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.41
_cell_measurement_theta_min      2.21
_cell_volume                     3731.5(2)
_computing_cell_refinement       X-Area
_computing_data_collection       X-Area
_computing_data_reduction        X-Area
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega 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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62518
_diffrn_reflns_theta_full        33.41
_diffrn_reflns_theta_max         33.41
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.406
_exptl_absorpt_correction_T_max  0.3750
_exptl_absorpt_correction_T_min  0.2184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.702
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.100
_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     497
_refine_ls_number_reflns         14354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0486P)^2^+3.7204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                9298
_reflns_number_total             14354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00199g.txt
_cod_data_source_block           shelxl6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7053062