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_4117051
_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, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl6 Co3 N12'
_chemical_formula_weight         1098.3
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n 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                   12.8145(9)
_cell_length_b                   13.955(1)
_cell_length_c                   11.1660(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     1996.8(3)
_computing_cell_refinement       'CAD4 V5'
_computing_data_collection       'CAD4 V5'
_computing_data_reduction        XCAD4
_computing_molecular_graphics    'SHELXTL V5 (Siemens, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       'omega - 2theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0086
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            1473
_diffrn_reflns_theta_max         22.43
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   'empirical via psi scan'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_description       block
_exptl_crystal_F_000             1110.
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(6)
_refine_ls_extinction_coef       0.0023(3)
_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   1.035
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         1449
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_obs          0.0325
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+5.9105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0836
_refine_ls_wR_factor_obs         0.0775
_reflns_number_observed          1265
_reflns_number_total             1449
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971997h_1.cif
_cod_data_source_block           cmpd_1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+5.9105P] 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^)+(0.0360P)^2^+5.9105P] 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_database_code               4117051