Organometallic Oxides: Oxidation of the Cubane [(η-C5R5)Cr(μ3-O)]4and the Structures and Magnetic Properties of the Salts {[(η-C5R5)Cr(μ3-O)]4}{tcnq} and {[(η-C5R5)Cr(μ3-O)]4}{BF4}
Allen, Daryl P.; Bottomley, Frank; Day, Robert W.; Decken, Andreas; Sanchez, Victor; Summers, David A.; Thompson, Robert C.; Organometallics 20 (2001) 1840–; doi:10.1021/om001067y

data_4084094
_publ_section_title
;
 Organometallic Oxides:&#x00A0; Oxidation of the Cubane
 [(\h-C5R5)Cr(\m3-O)]4and the Structures and Magnetic Properties of the
 Salts {[(\h-C5R5)Cr(\m3-O)]4}{tcnq} and {[(\h-C5R5)Cr(\m3-O)]4}{BF4}
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1840
_journal_paper_doi               10.1021/om001067y
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C54 H68 Cr4 N4 O4.5'
_chemical_formula_weight         1053.12
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_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                100.94(2)
_cell_angle_beta                 90.90(2)
_cell_angle_gamma                104.88(2)
_cell_formula_units_Z            2
_cell_length_a                   11.179(3)
_cell_length_b                   12.252(2)
_cell_length_c                   20.061(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2601.2(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.2011
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8879
_diffrn_reflns_theta_max         63.56
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    7.086
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             1104
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.155
_refine_ls_R_factor_all          0.2437
_refine_ls_R_factor_obs          0.0553
_refine_ls_shift/esd_max         -0.045
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2270
_refine_ls_wR_factor_obs         0.1379
_reflns_number_observed          2862
_reflns_number_total             8435
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om001067y.cif
_cod_data_source_block           '_CP*4Cr4O4TCNQ'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+4.0000P] 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^)+(0.0850P)^2^+4.0000P] 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        2601.2(11)
_cod_original_formula_sum        'C54 H68 Cr4 N4 O4.50'
_cod_database_code               4084094