The First Fused Dimer Metallacrown NiII2(mcpa)2(CH3OH)3(H2O)[12-MCNiIIN(shi)2(pko)2-4][12-MCNiIIN(shi)3(pko)-4]
George Psomas; Catherine Dendrinou-Samara; Maria Alexiou; Alexandros Tsohos; Catherine P. Raptopoulou; Aris Terzis; Dimitris P. Kessissoglou; Inorganic Chemistry 37 (1998) 6556–6557; doi:10.1021/ic980614t

data_4323251
_publ_section_title
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 The First Fused Dimer Metallacrown
 NiII2(mcpa)2(CH3OH)3(H2O)[12-MCNiIIN(shi)2(pko)2-4][12-MCNiIIN(shi)3(pko)-4]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6556
_journal_page_last               6557
_journal_paper_doi               10.1021/ic980614t
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C92.25 H89.4 Cl2 N14 Ni10 O32.45'
_chemical_formula_weight         2571.40
_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                106.41(2)
_cell_angle_beta                 100.20(1)
_cell_angle_gamma                99.81(2)
_cell_formula_units_Z            2
_cell_length_a                   21.691(9)
_cell_length_b                   16.843(8)
_cell_length_c                   17.767(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.5
_cell_volume                     5959(5)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15177
_diffrn_reflns_theta_max         22.30
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      1.41
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       'trigonal piece'
_exptl_crystal_F_000             2629
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.184
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         14759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.184
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_obs          0.0640
_refine_ls_shift/esd_max         0.069
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+28.6599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2180
_refine_ls_wR_factor_obs         0.1700
_reflns_number_observed          7956
_reflns_number_total             14759
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980614t.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+28.6599P] 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^)+(0.0837P)^2^+28.6599P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_formula_sum        'C92.25 H89.40 Cl2 N14 Ni10 O32.45'
_cod_database_code               4323251