Electrochemical synthesis and structural characterization of Co(II), Ni(II) and Cu(II) complexes of N,N-bis(4,5-dimethyl-2-hydroxybenzyl)-N-(2-pyridylmethyl)amine
Labisbal, Elena; Rodríguez, Laura; Souto, Oscar; Sousa-Pedrares, Antonio; García-Vázquez, José Arturo; Romero, Jaime; Sousa, Antonio; Yáñez, Matilde; Orallo, Francisco; Real, José A.; Dalton Transactions  (2009) 8644–8656; doi:10.1039/b907539a

data_7002436
_publ_section_title
;
 Electrochemical synthesis and structural characterization of Co(II),
 Ni(II) and Cu(II) complexes of
 N,N-bis(4,5-dimethyl-2-hydroxybenzyl)-N-(2-pyridylmethyl)amine
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8644
_journal_page_last               8656
_journal_paper_doi               10.1039/b907539a
_journal_year                    2009
_chemical_formula_sum            'C72 H78 N6 Ni3 O6'
_chemical_formula_weight         1299.53
_chemical_name_common
;
m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine, m3-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine, (m2, m3)-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-tri-nickel(ii)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.747(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   51.673(9)
_cell_length_b                   13.205(2)
_cell_length_c                   21.820(4)
_cell_measurement_reflns_used    1004
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.195
_cell_measurement_theta_min      2.915
_cell_volume                     14577(4)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            62460
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_correction_T_min  0.7464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G\"ottingen, Germany, 1996.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                11217
_reflns_number_total             14836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907539a.txt
_cod_data_source_block           Compound2
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7002436