Novel Rhenium(V) Oxo Complexes Containing Bis(pyrazol-1-yl)acetate and Bis(pyrazol-1-yl) Sulfonate as Tripodal N,N,O-heteroscorpionate Ligands
Marina Porchia; Grazia Papini; Carlo Santini; Giancarlo Gioia Lobbia; Maura Pellei; Francesco Tisato; Giuliano Bandoli; Alessandro Dolmella; Inorganic Chemistry 44 (2005) 4045–4054; doi:10.1021/ic050193x

data_4308926
_publ_section_title
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Novel Rhenium(V) Oxo Complexes Containing Bis(pyrazol-1-yl)acetate and
Bis(pyrazol-1-yl) Sulfonate as Tripodal N,N,O-heteroscorpionate Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4045
_journal_page_last               4054
_journal_paper_doi               10.1021/ic050193x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C7 H8 Cl3 N4 O Re'
_chemical_formula_weight         456.72
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.67(3)
_cell_angle_beta                 98.45(3)
_cell_angle_gamma                102.00(3)
_cell_formula_units_Z            2
_cell_length_a                   6.897(1)
_cell_length_b                   7.479(1)
_cell_length_c                   12.358(3)
_cell_measurement_temperature    293(2)
_cell_volume                     592.8(2)
_computing_cell_refinement
'X-RED Ver.1.22 (2001) STOE & Cie GmbH,Darmstadt'
_computing_data_collection
'CrysAlis Ver.1.169.9(release 21.05.02) Oxford Diffraction Ltd.'
_computing_data_reduction
'X-RED Ver.1.22 (2001) STOE & Cie GmbH,Darmstadt'
_computing_molecular_graphics    'SHELXTL NT Ver.5.10 (Bruker,1999)'
_computing_publication_material  'SHELXTL NT Ver.5.10 (Bruker,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT Ver.5.10 (Bruker,1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.766
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measurement_device_type  omega
_diffrn_measurement_method       'STADI4 CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2504
_diffrn_reflns_theta_full        29.32
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    10.907
_exptl_absorpt_correction_T_max  0.343
_exptl_absorpt_correction_T_min  0.052
_exptl_absorpt_correction_type   experimental
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.482
_refine_ls_extinction_coef       0.000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          1.324
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                2366
_reflns_number_total             2504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050193xsi20050204_043327_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4308926