Synthesis and Reactivity of Catecholate Complexes Containing Quadruply Bonded Metal Ions
Jason Christ; Corinne Epps; Victoria Pritchard; Derek Schmeh; Cortlandt Pierpont; Ebbe Nordlander; Inorganic Chemistry 49 (2010) 2029–2031; doi:10.1021/ic902328m

data_4315077
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Colorado
Boulder, CO  80309-0215
;
_publ_contact_author_email       pierpont@colorado.edu
_publ_contact_author_fax         '01 303 492 5894'
_publ_contact_author_name        'Professor Cortlandt Pierpont'
_publ_contact_author_phone       '01 303 492 8420'
_publ_section_title
;
 Synthesis and Reactivity of Catecholate Complexes Containing Quadruply
 Bonded Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2029
_journal_page_last               2031
_journal_paper_doi               10.1021/ic902328m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 Cl16 O8 Re2, 2(C6 H16 N), (C4 H8 O)'
_chemical_formula_sum            'C40 H40 Cl16 N2 O9 Re2'
_chemical_formula_weight         1632.41
_chemical_name_systematic
; 
 (HNEt3)2[Re2(Cl4C6O2)4](C4H8O) 
;
_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   calc
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.9220(10)
_cell_angle_beta                 66.4430(10)
_cell_angle_gamma                66.4270(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0186(3)
_cell_length_b                   13.7655(5)
_cell_length_c                   13.7710(5)
_cell_measurement_reflns_used    6438
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      30.437
_cell_measurement_theta_min      3.041
_cell_volume                     1735.81(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/XPREP'
_computing_molecular_graphics    'SHELXP (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      136(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0854
_diffrn_reflns_av_sigmaI/netI    0.1324
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12695
_diffrn_reflns_theta_full        29.37
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.14
_exptl_absorpt_correction_T_max  0.371
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
SQUEEZE was used to correct for the effect of the disordered THF
solvate located about an inversion center between two complex anions. 
;
_refine_diff_density_max         2.804
_refine_diff_density_min         -2.066
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.207
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2134
_reflns_number_gt                4856
_reflns_number_total             9082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902328m_si_001_2.cif
_cod_data_source_block           (HNEt3)2[Re2(Cl4C6O2)4](C4H8O)
_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^)+(0.1196P)^2^+0.0000P] 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^)+(0.1196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4315077