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_4117054
_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_structural     'Co3(dpa)4(BF4)2, 2(CH2Cl2)'
_chemical_formula_sum            'C42 H36 B2 Cl4 Co3 F8 N12'
_chemical_formula_weight         1201.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 114.76(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.594(2)
_cell_length_b                   13.754(4)
_cell_length_c                   18.937(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      9.1
_cell_volume                     4871(2)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL (Siemens, 1990)'
_computing_publication_material  'SHELXTL (Siemens, 1990)'
_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       'Frame data from omega 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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19422
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       plate
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         6361
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.069
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_obs          0.0700
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+60.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1686
_refine_ls_wR_factor_obs         0.1482
_reflns_number_observed          4989
_reflns_number_total             6364
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971997h_4.cif
_cod_data_source_block           cmpd_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+60.4235P] 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^)+(0.0229P)^2^+60.4235P] 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        4870.8(18)
_cod_database_code               4117054