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_4339632
_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         'C60 H36 Mn2 N24, 2(C2 H3 N), 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H46 Cl4 Mn2 N26'
_chemical_formula_weight         1454.97
_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                88.505(12)
_cell_angle_beta                 75.560(14)
_cell_angle_gamma                87.077(12)
_cell_formula_units_Z            1
_cell_length_a                   10.4432(17)
_cell_length_b                   12.2726(16)
_cell_length_c                   13.708(2)
_cell_measurement_reflns_used    3314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.40
_cell_measurement_theta_min      2.28
_cell_volume                     1699.0(4)
_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  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1988)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0994
_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            11335
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         4.09
_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    0.592
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         5953
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0876P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1827
_reflns_number_gt                3910
_reflns_number_total             5953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700590c_si_1.cif
_cod_data_source_block           cs781
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1698.9(4)
_cod_database_code               4339632