Linear Tricobalt Compounds with Di(2-pyridyl)amide (dpa) Ligands: Temperature Dependence of the Structural and Magnetic Properties of Symmetrical and Unsymmetrical Forms of Co3(dpa)4Cl2 in the Solid State
Rodolphe Clérac; F. Albert Cotton; Lee M. Daniels; Kim R. Dunbar; Kristin Kirschbaum; Carlos A. Murillo; A. Alan Pinkerton; Arthur J. Schultz; Xiaoping Wang; Journal of the American Chemical Society 122 (2000) 6226–6236; doi:10.1021/ja000515q

data_4116060
_publ_contact_author_address
; Dept. of Chemistry
  P.O. Box 30012
  Texas A&M University
  College Station, TX 77842-3012
  USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(409) 845 9351'
_publ_contact_author_name        'F.A. Cotton'
_publ_contact_author_phone       '(409) 845 4432'
_publ_section_title
;
 Linear Tricobalt Compounds with Di(2-pyridyl)amide (dpa) Ligands:
 Temperature Dependence of the Structural and Magnetic Properties of
 Symmetrical and Unsymmetrical Forms of Co3(dpa)4Cl2 in the Solid State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6226
_journal_page_last               6236
_journal_paper_doi               10.1021/ja000515q
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_structural     'Co3(dpa)4Cl2 2CH2Cl2'
_chemical_formula_sum            'C42 H36 Cl6 Co3 N12'
_chemical_formula_weight         1098.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            8
_cell_length_a                   27.004(4)
_cell_length_b                   27.004(4)
_cell_length_c                   12.230(2)
_cell_measurement_reflns_used    689
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.80
_cell_volume                     8918(2)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20(2)
_diffrn_measurement_device       'SMART 2000'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35003
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       columnar
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0416
_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^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0952
_refine_ls_wR_factor_obs         0.0903
_reflns_number_observed          10441
_reflns_number_total             12528
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja000515q_1.cif
_cod_data_source_block           u20K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] 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^)+(0.0402P)^2^+0.0000P] 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        8918.3(24)
_cod_database_code               4116060