A compound of a novel tetraaza-macrocycle with trinuclear tetracyanonickelate-bridged cations
Neil F. Curtis; Horst Puschman; Acta Crystallographica Section C 60 (2004) m410–m413; doi:10.1107/S0108270104015483

data_2014211
_publ_section_title
;
 A compound of a novel tetraaza-macrocycle with trinuclear
 tetracyanonickelate-bridged cations
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m410
_journal_page_last               m413
_journal_paper_doi               10.1107/S0108270104015483
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
;
[Cu2 Ni (C N)4 (C15 H31 N5 O2)2 (H2 O)2] [Cu2 Ni (C N)4 (C15 H31 N5 O2)2]
[Ni (C N)4]2, 8H2 O
;
_chemical_formula_moiety
'C34 H66 Cu2 N14 Ni O6 2+, C34 H62 Cu2 N14 Ni O4 2+, 2C4 N4 Ni 2-, 8H2 O'
_chemical_formula_sum            'C76 H144 Cu4 N36 Ni4 O18'
_chemical_formula_weight         2339.23
_chemical_name_systematic
;
di-\m-cyano-1:2\k^2^C:N;1:3\k^2^C:N-tetracyano-1\k^4^N-bis(13-ethyl-5,7,7-
trimethyl-13-nitro-1,4,8,11-tetraazacyclotetradec-4-ene)-
2\k^4^N^1^,N^4^,N^8^,N^11^;3\k^4^N^1^,N^4^,N^8^,N^11^-dicopper(II)nickel(II)
diaqua-1,3\k^2^O-di-\m-cyano-1:2\k^2^C:N;1:3\k^2^C:N-tetracyano-1\k^4^N-
bis(13-ethyl-5,7,7-trimethyl-13-nitro-1,4,8,11-tetraazacyclotetradec-4-ene)-
2\k^4^N^1^,N^4^,N^8^,N^11^;3\k^4^N^1^,N^4^,N^8^,N^11^-dicopper(II)nickel(II)
bis[tetracyanonickelate(II)] octahydrate
;
_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                70.1540(10)
_cell_angle_beta                 78.1650(10)
_cell_angle_gamma                81.2900(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7497(2)
_cell_length_b                   14.0540(3)
_cell_length_c                   17.9014(4)
_cell_measurement_reflns_used    7862
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.267
_cell_measurement_theta_min      2.250
_cell_volume                     2710.63(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3.2 (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22241
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.1
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
R(int)=0.0470 before correction
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.734
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         14372
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+5.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                9857
_reflns_number_total             14372
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1674.cif
_cod_data_source_block           I
_cod_original_cell_volume        2710.60(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2014211
_cod_database_fobs_code          2014211