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_7027384
_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            'C47 H38 Cl2 N10 Ni2 O8'
_chemical_formula_weight         1059.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.00(3)
_cell_angle_beta                 84.61(3)
_cell_angle_gamma                63.04(3)
_cell_formula_units_Z            2
_cell_length_a                   12.739(3)
_cell_length_b                   14.266(3)
_cell_length_c                   14.699(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2319.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.561
_diffrn_measured_fraction_theta_max 0.561
_diffrn_measurement_device_type  CAD-4
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  beta-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3603
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        .7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.9072
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            crimson
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+1.7669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                3391
_reflns_number_total             3391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902018gsup1.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+1.7669P] 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^)+(0.0751P)^2^+1.7669P] 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        2319.9(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027384