Pyridine Ring Opening at Room Temperature at a Rhenium Tricarbonyl Bipyridine Complex
Miguel A. Huertos; Julio Pérez; Lucía Riera; Journal of the American Chemical Society 130 (2008) 5662–5663; doi:10.1021/ja801655d

data_4107734
_publ_contact_author_address
;
     Departamento de Quimica Organica e Inorganica
     IUQOEM - Facultad de Quimica
     Universidad de Oviedo-CSIC
     C/ Julian Claveria s/n
     33006 Oviedo  (ASTURIAS)
     SPAIN
;
_publ_contact_author_email       'japm@uniovi.es, lrm@fq.uniovi.es'
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-102985
_publ_section_title
;
 Pyridine Ring Opening at Room Temperature at a Rhenium Tricarbonyl
 Bipyridine Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5662
_journal_page_last               5663
_journal_paper_doi               10.1021/ja801655d
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_sum            'C32 H30 Cl6 F3 N4 O6 Re S'
_chemical_formula_weight         1054.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            8
_cell_length_a                   11.49680(10)
_cell_length_b                   24.9690(2)
_cell_length_c                   27.7281(2)
_cell_measurement_reflns_used    25721
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6295
_cell_measurement_theta_min      3.1826
_cell_volume                     7959.73(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
;
_computing_molecular_graphics    X-Seed
_computing_publication_material  X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.938
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34865
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         73.84
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    10.706
_exptl_absorpt_correction_T_max  0.425
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.373
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         13723
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+82.8433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                13203
_reflns_number_total             13723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801655d-file004_2.cif
_cod_data_source_block           COMPOUND_3d_(ma215)
_cod_database_code               4107734