Tetranuclear Copper(II) and Nickel(II) Cluster Complexes Derived by Self-Assembly from a Series of Tetradentate Diazine Ligands: Structural and Magnetic Studies
Craig J. Matthews; Karen Avery; Zhiqiang Xu; Laurence K. Thompson; Liang Zhao; David O. Miller; Kumar Biradha; Karen Poirier; Michael J. Zaworotko; Claire Wilson; Andrés E. Goeta; Judith A. K. Howard; Inorganic Chemistry 38 (1999) 5266–5276; doi:10.1021/ic990598f

data_4322399
_publ_section_title
;
 Tetranuclear Copper(II) and Nickel(II) Cluster Complexes Derived by
 Self-Assembly from a Series of Tetradentate Diazine Ligands: Structural
 and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5266
_journal_page_last               5276
_journal_paper_doi               10.1021/ic990598f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C48 H53 N23.5 Ni4 O24.5'
_chemical_formula_weight         1585.98
_chemical_name_systematic
; 
 ? 
;
_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                93.1050(10)
_cell_angle_beta                 100.1500(10)
_cell_angle_gamma                108.5050(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0509(6)
_cell_length_b                   12.7498(6)
_cell_length_c                   23.1208(11)
_cell_measurement_temperature    193(2)
_cell_volume                     3292.9(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17183
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.222
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             1627
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.261
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.0015(4)
_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   1.030
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         10806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_obs          0.0659
_refine_ls_shift/esd_max         3.155
_refine_ls_shift/esd_mean        0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+14.2648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2171
_refine_ls_wR_factor_obs         0.1992
_reflns_number_observed          8641
_reflns_number_total             11223
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990598f_3.cif
_cod_data_source_block           Ka05c(6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+14.2648P] 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^)+(0.1305P)^2^+14.2648P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C48 H53 N23.50 Ni4 O24.50'
_cod_database_code               4322399