New Synthetic Routes to Cationic Rhenium Tricarbonyl Bipyridine Complexes with Labile Ligands
Eva Hevia; Julio Pérez; Víctor Riera; Daniel Miguel; Scott Kassel; Arnold Rheinghold; Inorganic Chemistry 41 (2002) 4673–4679; doi:10.1021/ic020174c

data_4318437
_publ_contact_author
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     JULIO PEREZ
     Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu\'imica
     Universidad de Oviedo
     C/ Julian Claveria s/n
     33006 Oviedo  (ASTURIAS)
     SPAIN
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_publ_contact_author_email       japm@sauron.quimica.uniovi.es
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-102985
_publ_section_title
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 New Synthetic Routes to Cationic Rhenium Tricarbonyl Bipyridine Complexes
 with Labile Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4673
_journal_page_last               4679
_journal_paper_doi               10.1021/ic020174c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C53 H28 B F24 N2 O4 Re'
_chemical_formula_weight         1409.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.181(6)
_cell_length_b                   15.957(6)
_cell_length_c                   20.129(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5519(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34647
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.633550
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(8)
_refine_ls_extinction_coef       0.00013(5)
_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   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         7941
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.087
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+17.7319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                6578
_reflns_number_total             7941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020174c_3.cif
_cod_data_source_block           Compound_6b_(ehf1def)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        5518(3)
_cod_database_code               4318437