Synthesis, redox chemistry and EPR spectroscopy of the mixed-sandwich complexes (η-arene)(η-cycloheptatrienyl)metal(z+) (M = Cr or Mo; z = 1 or 2): crystal structures of the redox pair [Cr(η-C6H5Me)(η-C7H6C6H4Me-4)][PF6]n (n = 1 or 2)
Beddoes, Roy L.; Elwell, Mark S.; Mabbs, Frank E.; McInnes, Eric J. L.; Roberts, Andrew; Sarwar, M. Fahad; Whiteley, Mark W.; Journal of the Chemical Society, Dalton Transactions  (2000) 4669–; doi:10.1039/b007830l

data_7010294
_publ_contact_author
;
Mark Whiteley
Dept. Chem. Univ. of Manchester
;
_publ_section_title
;
 Synthesis, redox chemistry and EPR spectroscopy of the mixed-sandwich
 complexes (\h-arene)(\h-cycloheptatrienyl)metal(z+)
 (M&#x2005;=&#x2005;Cr or Mo; z&#x2005;=&#x2005;1 or 2): crystal
 structures of the redox pair [Cr(\h-C6H5Me)(\h-C7H6C6H4Me-4)][PF6]n
 (n&#x2005;=&#x2005;1 or 2)
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4669
_journal_paper_doi               10.1039/b007830l
_journal_year                    2000
_chemical_formula_sum            'C21 H21 Cr F6 P'
_chemical_formula_weight         470.36
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             19100-09-26
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.019(3)
_cell_length_b                   27.297(8)
_cell_length_c                   11.095(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    295.2
_cell_measurement_theta_max      9.8
_cell_measurement_theta_min      7.7
_cell_volume                     3942.9(18)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_diffrn_ambient_temperature      295.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.07517
_diffrn_orient_matrix_UB_12      -0.00109
_diffrn_orient_matrix_UB_13      -0.01838
_diffrn_orient_matrix_UB_21      -0.00015
_diffrn_orient_matrix_UB_22      0.03630
_diffrn_orient_matrix_UB_23      -0.01209
_diffrn_orient_matrix_UB_31      0.01580
_diffrn_orient_matrix_UB_32      -0.00480
_diffrn_orient_matrix_UB_33      -0.08740
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.090
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3893
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0.14
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1920.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.762
_refine_ls_goodness_of_fit_obs   3.402
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_obs          0.0622
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0471
_refine_ls_wR_factor_obs         0.0450
_reflns_number_observed          2173
_reflns_number_total             3893
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b007830l.txt
_cod_data_source_block           S513
_cod_depositor_comments
;
 Homogenising atom site labels in order to relate data from different loops.

 Antanas Vaitkus,
 2018-08-08

 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo)' 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)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3943(1)
_cod_original_sg_symbol_H-M      'P b c a    '
_cod_original_formula_sum        'C21 H21 Cr F6 P '
_cod_database_code               7010294