A New Linear Tricobalt Compound with Di(2-pyridyl)amide (dpa) Ligands: Two-Step Spin Crossover of [Co3(dpa)4Cl2][BF4]
Rodolphe Clérac; F. Albert Cotton; Kim R. Dunbar; Tongbu Lu; Carlos A. Murillo; Xiaoping Wang; Journal of the American Chemical Society 122 (2000) 2272–2278; doi:10.1021/ja994051b

data_4115951
_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
;
 A New Linear Tricobalt Compound with Di(2-pyridyl)amide (dpa) Ligands:
 Two-Step Spin Crossover of [Co3(dpa)4Cl2][BF4]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2272
_journal_page_last               2278
_journal_paper_doi               10.1021/ja994051b
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_structural     '[Co3(dpa)4Cl2][BF4]1.5CH2Cl2'
_chemical_formula_sum            'C41.5 H35 B Cl5 Co3 F4 N12'
_chemical_formula_weight         1142.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.061(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3249(7)
_cell_length_b                   20.759(1)
_cell_length_c                   19.422(1)
_cell_measurement_reflns_used    4221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.94
_cell_measurement_theta_min      4.52
_cell_volume                     4559.5(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device       'SMART CCD 1000'
_diffrn_measurement_method       '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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25447
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       plates
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.328
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.248
_refine_ls_hydrogen_treatment    nonref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         8936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.248
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         -0.027
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1484
_refine_ls_wR_factor_obs         0.1337
_reflns_number_observed          6286
_reflns_number_total             8940
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja994051b_2.cif
_cod_data_source_block           100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+17.0000P] 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^)+(0.0460P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_formula_sum        'C41.50 H35 B Cl5 Co3 F4 N12'
_cod_database_code               4115951