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_4116065
_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_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                   27.189(1)
_cell_length_b                   27.189(1)
_cell_length_c                   12.2293(7)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      9.05
_cell_volume                     9040.4(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19540
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.490
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.614
_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         0.737
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.081
_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   1.022
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_obs          0.0378
_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^)+(0.0242P)^2^+70.0886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0920
_refine_ls_wR_factor_obs         0.0902
_reflns_number_observed          5872
_reflns_number_total             6067
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja000515q_6.cif
_cod_data_source_block           u173K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+70.0886P] 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^)+(0.0242P)^2^+70.0886P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116065