Symmetrical and Unsymmetrical Compounds Having a Linear Co36+ Chain Ligated by a Spiral Set of Dipyridyl Anions
F. Albert Cotton; Lee M. Daniels; Glenn T. Jordan; Carlos A. Murillo; Journal of the American Chemical Society 119 (1997) 10377–10381; doi:10.1021/ja971997h

data_4117052
_publ_section_title
;
 Symmetrical and Unsymmetrical Compounds Having a Linear Co36+ Chain
 Ligated by a Spiral Set of Dipyridyl Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10377
_journal_page_last               10381
_journal_paper_doi               10.1021/ja971997h
_journal_volume                  119
_journal_year                    1997
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C20 H16 Co N6'
_chemical_formula_sum            'C60 H48 Cl2 Co4 N18'
_chemical_formula_weight         1327.8
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.803(8)
_cell_length_b                   13.803(2)
_cell_length_c                   14.9460(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      41.6
_cell_measurement_theta_min      18.1
_cell_volume                     2847.6(17)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5 (Siemens, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'area detector'
_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  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16847
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green-brown'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       'large sphere'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_obs          0.0393
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.2324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_obs         0.0908
_reflns_number_observed          2111
_reflns_number_total             2532
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971997h_2.cif
_cod_data_source_block           cmpd_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.2324P] 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^)+(0.0346P)^2^+4.2324P] 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        2848(2)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4117052