Electrochemical synthesis and structural characterisation of transition metal complexes with 2,6-bis(1-salicyloylhydrazonoethyl)pyridine, H4daps
Bermejo, Manuel R.; Fondo, Matilde; González, Ana M.; Hoyos, Olga L.; Sousa, Antonio; McAuliffe, Charles A.; Hussain, Wasif; Pritchard, Robin; Novotorsev, Vladimir M.; Journal of the Chemical Society, Dalton Transactions  (1999) 2211–; doi:10.1039/a902018g

data_7027385
_publ_section_title
;
 Electrochemical synthesis and structural characterisation of transition
 metal complexes with 2,6-bis(1-salicyloylhydrazonoethyl)pyridine, H4daps
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2211
_journal_paper_doi               10.1039/a902018g
_journal_year                    1999
_chemical_formula_sum            'C28.5 H25 Cl N6 Ni O4'
_chemical_formula_weight         609.70
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 122.32(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.993(4)
_cell_length_b                   20.649(4)
_cell_length_c                   16.821(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6162(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet P3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2791
_diffrn_reflns_theta_max         57.42
_diffrn_reflns_theta_min         6.23
_diffrn_standards_decay_%        51
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.135
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.838
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0014(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.826
_refine_ls_goodness_of_fit_obs   0.827
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         2791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_restrained_S_obs      0.827
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_obs          0.1232
_refine_ls_shift/esd_max         1.651
_refine_ls_shift/esd_mean        0.620
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3265P)^2^+68.8911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3253
_refine_ls_wR_factor_obs         0.3245
_reflns_number_observed          2772
_reflns_number_total             2791
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902018gsup1.cif
_cod_data_source_block           4
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.3265P)^2^+68.8911P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.3265P)^2^+68.8911P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6162.0(20)
_cod_original_sg_symbol_H-M      'C2/c (No 15)'
_cod_original_formula_sum        'C28.50 H25 Cl N6 Ni O4'
_cod_database_code               7027385