Compounds with Symmetrical Tricobalt Chains Wrapped by Dipyridylamide Ligands and Cyanide or Isothiocyanate Ions as Terminal Ligands
Rodolphe Clérac; F. Albert Cotton; Stephen P. Jeffery; Carlos A. Murillo; Xiaoping Wang; Inorganic Chemistry 40 (2001) 1265–1270; doi:10.1021/ic001069a

data_4319417
_publ_section_title
;
 Compounds with Symmetrical Tricobalt Chains Wrapped by Dipyridylamide
 Ligands and Cyanide or Isothiocyanate Ions as Terminal Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1265
_journal_page_last               1270
_journal_paper_doi               10.1021/ic001069a
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesis
_chemical_formula_structural     Co3(dpa)4(SCN)2.1.5CH2Cl2
_chemical_formula_sum            'C43.5 H35 Cl3 Co3 N14 S2'
_chemical_formula_weight         1101.12
_chemical_name_systematic
; 
 ? 
;
_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                 106.782(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9200(10)
_cell_length_b                   17.6210(10)
_cell_length_c                   16.2104(9)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     4627.2(5)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27597
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_obs          0.0453
_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^)+(0.0454P)^2^+8.3527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1163
_refine_ls_wR_factor_obs         0.1075
_reflns_number_observed          7048
_reflns_number_total             8124
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001069a_3.cif
_cod_data_source_block           5.1.5CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+8.3527P] 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^)+(0.0454P)^2^+8.3527P] 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        'C43.50 H35 Cl3 Co3 N14 S2'
_cod_database_code               4319417