Metal Complexes of Bridging Neutral Radical Ligands: pymDTDA and pymDSDA
Jian Wu; Daniel J. MacDonald; Rodolphe Clérac; Ie-Rang Jeon; Michael Jennings; Alan J. Lough; James Britten; Craig Robertson; Paul A. Dube; Kathryn E. Preuss; Inorganic Chemistry 51 (2012) 3827–3839; doi:10.1021/ic3000284

data_4328701
_publ_section_title
;
 Metal Complexes of Bridging Neutral Radical Ligands: pymDTDA and pymDSDA
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3827
_journal_page_last               3839
_journal_paper_doi               10.1021/ic3000284
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C25 H7 F24 N4 Ni2 O8 Se2'
_chemical_formula_sum            'C25 H7 F24 N4 Ni2 O8 Se2'
_chemical_formula_weight         1222.69
_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                67.20(3)
_cell_angle_beta                 70.41(3)
_cell_angle_gamma                85.75(3)
_cell_formula_units_Z            2
_cell_length_a                   10.620(2)
_cell_length_b                   14.630(3)
_cell_length_c                   14.893(3)
_cell_measurement_reflns_used    31936
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2005.5(9)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30490
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7088
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0960P)^2^+3.3240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1773
_reflns_number_gt                4754
_reflns_number_total             7088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3000284_si_001_03.cif
_cod_data_source_block           2b
_cod_original_cell_volume        2005.5(7)
_cod_database_code               4328701