Electrochemical synthesis and structural characterization of homoleptic and heteroleptic cobalt, nickel, copper, zinc and cadmium compounds with the 2-hydroxy-1,4-naphthoquinone ligand
Casanova, Isabel; Sousa-Pedrares, Antonio; Viqueira, Joaquin; Durán, María L.; Romero, Jaime; Sousa, Antonio; García-Vázquez, José A.; New Journal of Chemistry 37 (2013) 2303–; doi:10.1039/c3nj00227f

data_7053076
_publ_section_title
;
 Electrochemical synthesis and structural characterization of homoleptic
 and heteroleptic cobalt, nickel, copper, zinc and cadmium compounds with
 the 2-hydroxy-1,4-naphthoquinone ligand
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2303
_journal_paper_doi               10.1039/c3nj00227f
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C30 H18 Co N2 O6'
_chemical_formula_weight         561.39
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.554(4)
_cell_length_b                   14.761(3)
_cell_length_c                   8.3825(16)
_cell_measurement_reflns_used    868
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.84
_cell_measurement_theta_min      2.76
_cell_volume                     2419.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1463
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6642
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.8268
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2095
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                1049
_reflns_number_total             2095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00227f.txt
_cod_data_source_block           isa0310
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_database_code               7053076