N-(2-Mercaptoethyl)picolylamine as a Diaminomonothiolate Ligand for the "fac-[Re(CO)3]+" Core
Daniel J. Kramer; Alan Davison; William M. Davis; Alun G. Jones; Inorganic Chemistry 41 (2002) 6181–6183; doi:10.1021/ic025887+

data_4327547
_publ_section_title
;
 N-(2-Mercaptoethyl)picolylamine as a Diaminomonothiolate Ligand for the
 "fac-[Re(CO)3]+" Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6181
_journal_page_last               6183
_journal_paper_doi               10.1021/ic025887+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Re(CO)3(MEPA-NEt)
_chemical_formula_sum            'C13 H15 N2 O3 Re S'
_chemical_formula_weight         465.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.7240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2999(4)
_cell_length_b                   14.9969(8)
_cell_length_c                   13.5499(8)
_cell_measurement_reflns_used    6031
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.82
_cell_volume                     1469.93(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      183(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  0.1225
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5514
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    8.416
_exptl_absorpt_correction_T_max  0.5909
_exptl_absorpt_correction_T_min  0.2536
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.755
_refine_diff_density_min         -2.636
_refine_diff_density_rms         0.230
_refine_ls_extinction_coef       0.0010(3)
_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   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0447P)^2^+4.2988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                1870
_reflns_number_total             1921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0258872B_s2_2.cif
_cod_data_source_block           02121m
_cod_database_code               4327547