Nickel(II)-Dipeptidoamine-Based Tetrameric Complex: Structural Study in Solution and in Solid State
Katalin Selmeczi; Patrick Gizzi; Delphine Champmartin; Patrice Rubini; Emmanuel Aubert; Slimane Dahaoui; Bernard Henry; Inorganic Chemistry 49 (2010) 8222–8229; doi:10.1021/ic101167f

data_4316547
_publ_contact_author_address
;
Laboratoire SRSMC (UMR CNRS - Universit\'e Henri Poincar\'e 
Nancy 1), Nancy Universit\'e, BP 239, F-54506 Vandoeuvre-l\`es-Nancy Cedex,
France
;
_publ_contact_author_email       katalin.selmeczi@srsmc.uhp-nancy.fr
_publ_contact_author_fax         '0033 (0)3 83 68 43 22'
_publ_contact_author_name        'Katalin SELMECZI'
_publ_contact_author_phone       '0033 (0)3 83 68 43 38'
_publ_section_title
;
 Nickel(II)-Dipeptidoamine-Based Tetrameric Complex: Structural Study in
 Solution and in Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8222
_journal_page_last               8229
_journal_paper_doi               10.1021/ic101167f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H56 N16 Ni4 O4, 4.5CH3OH, 1.5H2O'
_chemical_formula_sum            'C40.5 H77 N16 Ni4 O10'
_chemical_formula_weight         1182.92
_chemical_name_common            Ni4(alphaMeAla-Histamine)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2645(4)
_cell_length_b                   23.5003(8)
_cell_length_c                   20.9007(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5405.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23958
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.985
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         12358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.130
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+18.8285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                8441
_reflns_number_total             12358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101167f_si_002.cif
_cod_data_source_block           tetra_10
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316547