Structure of the Chromium(III) Salt [Cp^*^~2~Cr]^+^[Cp^*^CrCl~3~]^{-^}
Aldridge, Simon; Shang, Maoyu; Fehlner, Thomas P.; Acta Crystallographica Section C 54 (1998) 47–49; doi:10.1107/S0108270197011256

data_2006928
_publ_section_title
;
 Structure of the Chromium(III) Salt [Cp^*^~2~Cr]^+^[Cp^*^CrCl~3~]^{-^}
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              47
_journal_page_last               49
_journal_paper_doi               10.1107/S0108270197011256
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Cr(C10 H15)2][CrCl3 (C10 H15)]'
_chemical_formula_sum            'C30 H45 Cl3 Cr2'
_chemical_formula_weight         616.01
_chemical_name_systematic
;
Bis(\h^5^-Pentamethylcyclopentadienyl)chromium(III) (\h^5^-
Pentamethylcyclopentadienyl)trichlorochromium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.289(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.602(2)
_cell_length_b                   13.0428(10)
_cell_length_c                   19.074(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13
_cell_volume                     3126.3(7)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1977)'
_computing_data_reduction        'SDP (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5736
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        12.3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'Very dark green'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bar
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.256
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.153
_refine_ls_goodness_of_fit_obs   1.167
_refine_ls_hydrogen_treatment    'see text below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_obs          .0528
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0439P)^2^+5.8729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1467
_refine_ls_wR_factor_obs         .1290
_reflns_number_observed          4242
_reflns_number_total             5480
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fr1067.cif
_cod_data_source_block           f9701
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0439P)^2^+5.8729P] 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^)+(0.0439P)^2^+5.8729P] 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        3126.4(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2006928