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_7002437
_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            'C49 H58.5 N4.5 Ni2 O6.5'
_chemical_formula_weight         931.92
_chemical_name_common
;
bis-(m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-(aqua) di-nickel(ii) acetonitrile solvate
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.000(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.083(6)
_cell_length_b                   17.120(7)
_cell_length_c                   19.394(8)
_cell_measurement_reflns_used    795
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.38
_cell_measurement_theta_min      2.38
_cell_volume                     4537(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1172
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38942
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8641
_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    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9334
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                4814
_reflns_number_total             9334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907539a.txt
_cod_data_source_block           Compound3
_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      P2(1)/n
_cod_original_formula_sum        'C49 H58.50 N4.50 Ni2 O6.50'
_cod_database_code               7002437