TCNE dimer dianion coordination complexes, [Mn(TPA)(TCNE)]2[micro2-(TCNE)2] and [Mn(TPA)(micro4-C4(CN)8)0.5].ClO4, TPA=tris(2-pyridylmethyl)amine: synthesis, structure and magnetic properties.
Wang, Guangbin; Slebodnick, Carla; Yee, Gordon T.; Inorganic chemistry 46 (2007) 9641–9645; doi:10.1021/ic700590c

data_4339633
_publ_section_title
;
 TCNE dimer dianion coordination complexes,
 [Mn(TPA)(TCNE)]2[micro2-(TCNE)2] and [Mn(TPA)(micro4-C4(CN)8)0.5].ClO4,
 TPA=tris(2-pyridylmethyl)amine: synthesis, structure and magnetic
 properties.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9641
_journal_page_last               9645
_journal_paper_doi               10.1021/ic700590c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C24 H18 Mn N8, Cl O4'
_chemical_formula_sum            'C24 H18 Cl Mn N8 O4'
_chemical_formula_weight         572.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           94
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4n 2n'
_symmetry_space_group_name_H-M   'P 42 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.170(3)
_cell_length_b                   17.170(3)
_cell_length_c                   17.1837(6)
_cell_measurement_reflns_used    2407
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.32
_cell_measurement_theta_min      2.41
_cell_volume                     5065.9(13)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WinGX (Farrugia, 1999) and Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare,1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36863
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                3509
_reflns_number_total             4509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700590c_si_2.cif
_cod_data_source_block           cs929
_cod_database_code               4339633