Reactions of Diiminopyridine Ligands with Chalcogen Halides
Caleb D. Martin; Paul J. Ragogna; Inorganic Chemistry 51 (2012) 2947–2953; doi:10.1021/ic202213x

data_4328502
_publ_contact_author_address
;Department of Chemistry
The University of Western Ontario
Chemistry Building 1151 Richmond Street
London, Ontario, Canada N6A 5B7
;
_publ_contact_author_email       pragogna@uwo.ca
_publ_contact_author_fax         519-661-3022
_publ_contact_author_name        ' Paul J. Ragogna'
_publ_contact_author_phone       '519-661-2111 x87048'
_publ_section_title
;
 Reactions of Diiminopyridine Ligands with Chalcogen Halides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2947
_journal_page_last               2953
_journal_paper_doi               10.1021/ic202213x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C31 H39 N3 Se, 2(C2 H3 N), C2 N, Cl2 Se, 2(Cl)'
_chemical_formula_sum            'C37 H45 Cl4 N6 Se2'
_chemical_formula_weight         873.51
_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                 103.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.413(2)
_cell_length_b                   14.310(3)
_cell_length_c                   26.554(7)
_cell_measurement_reflns_used    15768
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     4225.6(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w 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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1196
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            16211
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.6408
_exptl_absorpt_correction_T_min  0.5803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                5267
_reflns_number_total             9628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202213x_si_002_2.cif
_cod_data_source_block           1SeCl
_cod_original_cell_volume        4225.6(16)
_cod_database_code               4328502