Template synthesis of square-planar nickel(II) and copper(III) complexes based on hydrazide ligands
Fritsky, Igor O.; Kozłowski, Henryk; Sadler, Peter J.; Yefetova, Oksana P.; Śwątek-Kozłowska, Jolanta; Kalibabchuk, Valentina A.; Głowiak, Tadeusz; Journal of the Chemical Society, Dalton Transactions  (1998) 3269–; doi:10.1039/a802451k

data_7028196
_publ_contact_author             'Igor O.Fritsky'
_publ_section_title
;
 Template synthesis of square-planar nickel(II) and copper(III) complexes
 based on hydrazide ligands
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3269
_journal_paper_doi               10.1039/a802451k
_journal_year                    1998
_chemical_formula_sum            'C9 H16 K N6 Ni O6.5'
_chemical_formula_weight         410.09
_chemical_name_systematic
; 
 Potassium {3,5-bis-(2'-hydroxyiminopropanoyl)-1,3,5-oxadiazinane 
 (3-)}nickolate(II)  sesquihydrate 
;
_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
_cell_angle_alpha                99.51(4)
_cell_angle_beta                 111.95(2)
_cell_angle_gamma                106.86(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0890(10)
_cell_length_b                   10.376(4)
_cell_length_c                   10.6400(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.8
_cell_measurement_theta_min      23.4
_cell_volume                     754.1(4)
_computing_publication_material  'ORTEP, 1964'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
'Enraf-Nonius FAST area detector diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta 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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3049
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         2.16
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.013
_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_hydrogen_treatment    'see experimental'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         1556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.150
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1066
_refine_ls_wR_factor_obs         0.0977
_reflns_number_observed          1209
_reflns_number_total             1559
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k802451sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] 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^)+(0.0531P)^2^+0.0000P] 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        754.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C9 H16 K N6 Ni O6.50'
_cod_database_code               7028196