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_4328706
_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 O8 S2 Zn2, 2(C15 H5 F12 N4 O4 S2 Zn)'
_chemical_formula_sum            'C55 H17 F48 N12 O16 S6 Zn4'
_chemical_formula_weight         2467.65
_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                 100.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.884(4)
_cell_length_b                   8.8599(18)
_cell_length_c                   23.216(5)
_cell_measurement_reflns_used    19157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     4018.5(15)
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32152
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.880
_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    2.039
_exptl_crystal_description       needle
_exptl_crystal_F_000             2414
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.093
_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     677
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0653P)^2^+5.4393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                4806
_reflns_number_total             7095
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3000284_si_001_08.cif
_cod_data_source_block           5a'
_cod_original_cell_volume        4018.4(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4328706