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

data_4328505
_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         'C43 H47 N3 S, 2(C H Cl3), 2(Cl)'
_chemical_formula_sum            'C45 H49 Cl8 N3 S'
_chemical_formula_weight         947.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.556(3)
_cell_angle_beta                 72.774(3)
_cell_angle_gamma                80.973(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5843(19)
_cell_length_b                   13.324(2)
_cell_length_c                   16.054(2)
_cell_measurement_reflns_used    46914
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.62
_cell_volume                     2433.1(6)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0997
_diffrn_reflns_av_sigmaI/netI    0.1513
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45136
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SAINT
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                4936
_reflns_number_total             10316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202213x_si_002_5.cif
_cod_data_source_block           3SCl
_cod_database_code               4328505