The First Example of Isomerization of a Dimetal Complex Involving the Switch of a Metal-Metal Bond Order from 3 to 0. Synthesis and Characterization of the Paramagnetic Mixed-Valence Complex Cation [(XylNC)(OC)Re(μ-Cl)2(μ-dppm)2ReCl(CNXyl)]+1
Wengan Wu; Phillip E. Fanwick; Richard A. Walton; Journal of the American Chemical Society 118 (1996) 13091–13092; doi:10.1021/ja962910f

data_4117226
_publ_contact_author
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     Richard A. Walton
     Department of Chemistry
     Purdue University
     W. Lafayette
     IN 47907
     USA
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_publ_contact_author_email       ritab@purdue.edu
_publ_contact_author_fax         '(317) 494 0239'
_publ_contact_author_phone       '(317) 494 5464'
_publ_section_title
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 The First Example of Isomerization of a Dimetal Complex Involving the
 Switch of a Metal-Metal Bond Order from 3 to 0. Synthesis and
 Characterization of the Paramagnetic Mixed-Valence Complex Cation
 [(XylNC)(OC)Re(\m-Cl)2(\m-dppm)2ReCl(CNXyl)]+1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13091
_journal_page_last               13092
_journal_paper_doi               10.1021/ja962910f
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C87.21 Cl3.29 F2.13 N2 O3.13 P4 Re2 S0.71'
_chemical_formula_weight         1884.29
_chemical_name_systematic        ' ?'
_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_type_scat_source
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_audit_creation_date             12-02-96
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' JA962910F-240'
_cell_angle_alpha                80.27(4)
_cell_angle_beta                 65.06(4)
_cell_angle_gamma                83.72(4)
_cell_formula_units_Z            2
_cell_length_a                   15.751(7)
_cell_length_b                   16.645(7)
_cell_length_c                   18.886(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223
_cell_measurement_theta_max      25
_cell_measurement_theta_min      11
_cell_volume                     4421(4)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX93_(Sheldrick,_1993)
_computing_structure_solution    Patterson_and_Fourier
_diffrn_ambient_temperature      223
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       Enraf_Nonius_CAD4
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10996
_diffrn_reflns_theta_max         22.79
_diffrn_reflns_theta_min         3.01
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.022
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.2780
_exptl_absorpt_correction_type   refined_empirical_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.42
_exptl_crystal_description       plate
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.49
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    'not refined, U=1.3 * Ueq of bonding atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         10996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.070
_refine_ls_R_factor_obs          0.052
_refine_ls_shift/esd_max         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+48.8517P] where P=(Fo^2^+2Fc^2^)/'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.174
_refine_ls_wR_factor_obs         0.158
_reflns_number_observed          8815
_reflns_number_total             10996
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            ja962910f.cif
_cod_data_source_block           WU258W
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+48.8517P] where P=(Fo^2^+2Fc^2^)/' 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^)+(0.0969P)^2^+48.8517P] where P=(Fo^2^+2Fc^2^)/'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4117226