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_4318435
_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
;
 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            'C49 H28 B F24 N2 O4 Re'
_chemical_formula_weight         1361.74
_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                   16.849(4)
_cell_length_b                   16.734(4)
_cell_length_c                   18.467(5)
_cell_measurement_temperature    299(2)
_cell_volume                     5207(2)
_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      299(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32702
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.466
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.769985
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         7496
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                5854
_reflns_number_total             7496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020174c_1.cif
_cod_data_source_block           Compound_9_(thfa1)
_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_database_code               4318435