Hexaazamacrocyclic Nickel and Copper Complexes and their Reactivity with Tetracyanoquinodimethane
Loreto Ballester; Angel Gutiérrez; M. Felisa Perpiñán; Ana E. Sánchez; Marina Fonari; Maria Gdaniec; Inorganic Chemistry 46 (2007) 3946–3955; doi:10.1021/ic062016h

data_4307517
_publ_contact_author_address
;Departamento de Qu\'imica Inorg\'anica I
Facultad de Ciencias Qu\'imicas
Universidad Complutense
E-28040 Madrid
Spain
;
_publ_contact_author_email       alonso@quim.ucm.es
_publ_contact_author_fax         +34913944352
_publ_contact_author_name        'Angel Guti\'errez'
_publ_section_title
;
Hexaazamacrocyclic Nickel and Copper Complexes and their Reactivity with
Tetracyanoquinodimethane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3946
_journal_page_last               3955
_journal_paper_doi               10.1021/ic062016h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C60 H46 N22 Ni'
_chemical_formula_weight         1133.90
_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                78.04(3)
_cell_angle_beta                 86.39(3)
_cell_angle_gamma                76.43(3)
_cell_formula_units_Z            1
_cell_length_a                   8.805(2)
_cell_length_b                   12.308(2)
_cell_length_c                   13.052(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1345.0(5)
_computing_data_collection       'Lehman and Larsen, 1974'
_computing_data_reduction        'Lehman and Larsen, 1974'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  KM4CCD
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16320
_diffrn_reflns_theta_full        29.95
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_correction_T_min  0.8483
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0578
_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^)+(0.1271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                5850
_reflns_number_total             6973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062016h-file004_1.cif
_cod_data_source_block           NiN6TCNQ4_6
_cod_database_code               4307517