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_7051547
_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         'C18 H32 N6 Ni1, 2(Cl1 O4), C2 N1 H3'
_chemical_formula_sum            'C20 H35 Cl2 N7 Ni O8'
_chemical_formula_weight         631.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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             2005-09-27T08:47:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.313(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2314(11)
_cell_length_b                   12.7251(11)
_cell_length_c                   15.5407(12)
_cell_measurement_reflns_used    5802
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.546
_cell_measurement_wavelength     0.71073
_cell_volume                     2784.8(4)
_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    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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      -0.300337E-1
_diffrn_orient_matrix_UB_12      0.711362E-1
_diffrn_orient_matrix_UB_13      -0.13114E-2
_diffrn_orient_matrix_UB_21      -0.395223E-1
_diffrn_orient_matrix_UB_22      -0.232262E-1
_diffrn_orient_matrix_UB_23      0.447305E-1
_diffrn_orient_matrix_UB_31      0.507825E-1
_diffrn_orient_matrix_UB_32      0.239951E-1
_diffrn_orient_matrix_UB_33      0.47185E-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  0.046
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11072
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11072
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.1009
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+15.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2187
_reflns_number_gt                8922
_reflns_number_total             11072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b515107d.txt
_cod_data_source_block           new_3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7051547