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_7028195
_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            'C10 H22 Cu K0.5 Li0.5 N8 O11'
_chemical_formula_weight         516.92
_chemical_name_systematic
; 
(Lithium, potassium) {8,17-dioxa-1,2,5,6,10,11,14,15-octaazatricyclo
[13.3.1]eicosane-3,4,12,13-tetrone - (4-)} cuprate(III) pentahydrate
;
_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                 112.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.808(5)
_cell_length_b                   13.909(3)
_cell_length_c                   13.034(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.15
_cell_measurement_theta_min      9.8
_cell_volume                     3824.8(17)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3929
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.17
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.974
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    'see experimental'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_obs          0.0327
_refine_ls_shift/esd_max         0.390
_refine_ls_shift/esd_mean        0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0876
_refine_ls_wR_factor_obs         0.0796
_reflns_number_observed          2689
_reflns_number_total             3929
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k802451sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0461P)^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^)+(0.0461P)^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        3824.8(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C10 H22 Cu K0.50 Li0.50 N8 O11'
_cod_database_code               7028195