Intramolecular Nucleophilic Addition to the 2 Position of Coordinated 2,2'-Bipyridine by a Deprotonated Dimethyl Sulfide Ligand
Rebeca Arévalo; Julio Pérez; Lucía Riera; Inorganic Chemistry 52 (2013) 6785–6787; doi:10.1021/ic401065h

data_4335300
_publ_contact_author
;
     JULIO PEREZ 
     Departamento de Quimica Organica e Inorganica
     Facultad de Quimica
     Universidad de Oviedo
     C/ Julian Claveria 8
     33006 Oviedo  
     SPAIN
;
_publ_contact_author_email       japm@uniovi.es
_publ_contact_author_fax         +34-985103446
_publ_contact_author_phone       +34-985103465
_publ_section_title
;
 Intramolecular Nucleophilic Addition to the 2 Position of Coordinated
 2,2'-Bipyridine by a Deprotonated Dimethyl Sulfide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6785
_journal_page_last               6787
_journal_paper_doi               10.1021/ic401065h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C47 H26 B F24 N2 O3 Re S'
_chemical_formula_weight         1351.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   16.4783(2)
_cell_length_b                   18.2370(3)
_cell_length_c                   16.6378(3)
_cell_measurement_reflns_used    10226
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.426
_cell_measurement_theta_min      3.5933
_cell_volume                     4999.90(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14788
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    6.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.4007
_exptl_crystal_size_mid          0.0931
_exptl_crystal_size_min          0.0333
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+6.5201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                7114
_reflns_number_total             7556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401065h_si_001_3.cif
_cod_data_source_block           ra270-compound(1')
_cod_original_cell_volume        4999.9(1)
_cod_database_code               4335300