Reactions of α-Diimine Ligands with the in Situ Generated "S(OTf)2" Synthon
Caleb D. Martin; Paul J. Ragogna; Inorganic Chemistry 49 (2010) 4324–4330; doi:10.1021/ic100320u

data_4315418
_publ_contact_author_address
;Department of Chemistry
The University of Western Ontario
London, ON,
N6A 5B7, CANADA
;
_publ_contact_author_email       pragogna@uwo.ca
_publ_contact_author_fax         1(519)6613022
_publ_contact_author_name        'Paul J. Ragogna'
_publ_contact_author_phone       1(519)6612111x87048
_publ_section_title
;
 Reactions of \a-Diimine Ligands with the in Situ Generated "S(OTf)2"
 Synthon
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4324
_journal_page_last               4330
_journal_paper_doi               10.1021/ic100320u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C28 H20 F6 N2 O6 S3'
_chemical_formula_weight         690.64
_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                113.30(3)
_cell_angle_beta                 94.40(3)
_cell_angle_gamma                108.73(3)
_cell_formula_units_Z            2
_cell_length_a                   10.446(2)
_cell_length_b                   11.972(2)
_cell_length_c                   13.970(3)
_cell_measurement_reflns_used    12794
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1477.4(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_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 .999
_diffrn_measured_fraction_theta_max .999
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9435
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.8975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         .533
_refine_diff_density_min         -.532
_refine_diff_density_rms         .106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0754P)^2^+0.6709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                4145
_reflns_number_total             5230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100320u_si_001_4.cif
_cod_data_source_block           18
_cod_original_cell_volume        1477.4(5)
_cod_database_code               4315418