Nickel(ii) complexes of cyclen- and cyclam-pyridine: topological reorganisations induced by electron transfer
El Ghachtouli, Sanae; Cadiou, Cyril; Déchamps-Olivier, Isabelle; Chuburu, Françoise; Aplincourt, Michel; Patinec, Véronique; Le Baccon, Michel; Handel, Henri; Roisnel, Thierry; New Journal of Chemistry 30 (2006) 392–; doi:10.1039/b515107d

data_7051546
_publ_section_title
;
 Nickel(ii) complexes of cyclen- and cyclam-pyridine: topological
 reorganisations induced by electron transfer
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              392
_journal_paper_doi               10.1039/b515107d
_journal_volume                  30
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H28 N6 Ni1, 2(Cl O4)'
_chemical_formula_sum            'C16 H28 Cl2 N6 Ni O8'
_chemical_formula_weight         562.05
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-09-27T09:27:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6107(2)
_cell_length_b                   14.6567(2)
_cell_length_c                   21.6728(3)
_cell_measurement_reflns_used    5830
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.546
_cell_measurement_wavelength     0.71073
_cell_volume                     4641.11(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.172564E-1
_diffrn_orient_matrix_UB_12      0.524021E-1
_diffrn_orient_matrix_UB_13      0.271621E-1
_diffrn_orient_matrix_UB_21      -0.578449E-1
_diffrn_orient_matrix_UB_22      -0.82913E-2
_diffrn_orient_matrix_UB_23      0.240174E-1
_diffrn_orient_matrix_UB_31      0.322587E-1
_diffrn_orient_matrix_UB_32      -0.428995E-1
_diffrn_orient_matrix_UB_33      0.285369E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10038
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+3.2944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                4300
_reflns_number_total             5290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b515107d.txt
_cod_data_source_block           new_2
_cod_database_code               7051546