After 155 Years, A Crystalline Chromium Carboxylate with a Supershort Cr-Cr Bond
F. Albert Cotton; Elizabeth A. Hillard; Carlos A. Murillo; Hong-Cai Zhou; Journal of the American Chemical Society 122 (2000) 416–417; doi:10.1021/ja993755i

data_4115887
_publ_section_title
;
 After 155 Years, A Crystalline Chromium Carboxylate with a Supershort
 Cr-Cr Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              416
_journal_page_last               417
_journal_paper_doi               10.1021/ja993755i
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_moiety         'Cr2 (C16 H23 O2)4 (C2 H3 N)2,1.5(C H2 Cl2)'
_chemical_formula_structural     'Cr2 (TPB)4 (CH3CN)2,1.5(CH2Cl2)'
_chemical_formula_sum            'C69.5 H101 Cl3 Cr2 N2 O8'
_chemical_formula_weight         1302.87
_chemical_name_systematic
; 
 Cr2(TPB)4(CH3CN)2,1.5CH2Cl2 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                65.918(2)
_cell_angle_beta                 74.912(2)
_cell_angle_gamma                82.713(3)
_cell_formula_units_Z            2
_cell_length_a                   14.445(2)
_cell_length_b                   16.618(2)
_cell_length_c                   17.529(2)
_cell_measurement_reflns_used    8188
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.48
_cell_volume                     3708.1(8)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_diffrn_measurement_method       'Ellipsoid-mask Fitting'
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15829
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9638
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.147
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_obs          0.0909
_refine_ls_shift/esd_max         -0.080
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1858P)^2^+5.7332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3019
_refine_ls_wR_factor_obs         0.2656
_reflns_number_observed          6586
_reflns_number_total             9653
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993755i_3.cif
_cod_data_source_block           xl_compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1858P)^2^+5.7332P] 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^)+(0.1858P)^2^+5.7332P] 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        3708.1(9)
_cod_original_formula_sum        'C69.50 H101 Cl3 Cr2 N2 O8'
_cod_database_code               4115887