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_7051545
_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_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H31 N5 Ni1 O, 2(Cl O4)'
_chemical_formula_sum            'C16 H31 Cl2 N5 Ni O9'
_chemical_formula_weight         567.07
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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             2005-09-26T17:40:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4023(5)
_cell_length_b                   15.7925(5)
_cell_length_c                   16.3876(5)
_cell_measurement_reflns_used    65942
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.546
_cell_measurement_wavelength     0.71073
_cell_volume                     2433.33(17)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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      0.588443E-1
_diffrn_orient_matrix_UB_12      -0.45773E-2
_diffrn_orient_matrix_UB_13      0.506537E-1
_diffrn_orient_matrix_UB_21      0.101282E-1
_diffrn_orient_matrix_UB_22      0.63056E-1
_diffrn_orient_matrix_UB_23      0.14135E-2
_diffrn_orient_matrix_UB_31      -0.880296E-1
_diffrn_orient_matrix_UB_32      0.41951E-2
_diffrn_orient_matrix_UB_33      0.340226E-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  0.0534
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27402
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+1.4617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.124
_reflns_number_gt                4325
_reflns_number_total             5541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b515107d.txt
_cod_data_source_block           new1
_cod_database_code               7051545