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_4335298
_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            'C41.5 H46 Cl N2 O3 Re S'
_chemical_formula_weight         874.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 116.928(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.201(1)
_cell_length_b                   14.3041(3)
_cell_length_c                   24.6857(9)
_cell_measurement_reflns_used    8737
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      72.9938
_cell_measurement_theta_min      3.0868
_cell_volume                     8248.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.0(3)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34186
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         73.15
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    7.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.1375
_exptl_crystal_size_mid          0.0674
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.114
_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   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         16187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0577P)^2^+13.3733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                12857
_reflns_number_total             16187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401065h_si_001_1.cif
_cod_data_source_block           ra2722-compound6
_cod_original_cell_volume        8248.8(5)
_cod_database_code               4335298