Delocalized TCNQ Stacks in Nickel and Copper Tetraazamacrocyclic Systems
Loreto Ballester; Ana M. Gil; Angel Gutiérrez; M. Felisa Perpiñán; María Teresa Azcondo; Ana E. Sánchez; Eugenio Coronado; Carlos J. Gómez-García; Inorganic Chemistry 39 (2000) 2837–2842; doi:10.1021/ic9912070

data_4321097
_publ_contact_author
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Angel Gutierrez                                                        
Departamento de Quimica Inorganica I                                     
Facultad de Quimica                                         
Universidad Complutense                                                         
E-28040 Madrid                                                                  
Spain                                                                     
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_publ_contact_author_email       alonso@eucmax.sim.ucm.es
_publ_contact_author_fax         '+34 913944352'
_publ_contact_author_phone       '+34 913944337'
_publ_section_title
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 Delocalized TCNQ Stacks in Nickel and Copper Tetraazamacrocyclic Systems
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2837
_journal_page_last               2842
_journal_paper_doi               10.1021/ic9912070
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C52 H44 N16 Ni'
_chemical_formula_weight         951.74
_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
_cell_angle_alpha                103.038(12)
_cell_angle_beta                 101.23(2)
_cell_angle_gamma                109.37(2)
_cell_formula_units_Z            1
_cell_length_a                   8.809(2)
_cell_length_b                   10.896(2)
_cell_length_c                   13.727(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1157.7(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6646
_diffrn_reflns_theta_max         29.83
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.476
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             496
_refine_diff_density_max         1.515
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.0194(114)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.149
_refine_ls_goodness_of_fit_obs   1.438
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.438
_refine_ls_R_factor_all          0.2686
_refine_ls_R_factor_obs          0.052
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.5241
_refine_ls_wR_factor_obs         0.065
_reflns_number_observed          2596
_reflns_number_total             6646
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9912070_2.cif
_cod_data_source_block           '[Ni(transdieneN4)](TCNQ)3'
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.3003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.3003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1157.7(4)
_cod_database_code               4321097