Nuclearity of nickel and mixed sodium-nickel complexes: dependence on the spacer in chelating pyridine-alcoholate ligands.
Kayser, Laure; Pattacini, Roberto; Rogez, Guillaume; Braunstein, Pierre; Chemical communications (Cambridge, England) 46 (2010) 6461–6463; doi:10.1039/c0cc01425g

data_7112790
_publ_section_title
;
 Nuclearity of nickel and mixed sodium-nickel complexes: dependence on the
 spacer in chelating pyridine-alcoholate ligands.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6461
_journal_page_last               6463
_journal_paper_doi               10.1039/c0cc01425g
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C42 H49 N6 Ni3 O6, C H2 Cl2, Cl'
_chemical_formula_sum            'C43 H51 Cl3 N6 Ni3 O6'
_chemical_formula_weight         1030.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                74.300(1)
_cell_angle_beta                 82.417(1)
_cell_angle_gamma                65.885(1)
_cell_formula_units_Z            4
_cell_length_a                   15.2974(4)
_cell_length_b                   18.2533(5)
_cell_length_c                   21.4614(5)
_cell_measurement_reflns_used    48435
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     5264.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51917
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.26
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         24052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                15144
_reflns_number_total             24052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01425g.txt
_cod_data_source_block           Compound3
_cod_database_code               7112790