Artificial Amino Acids in Nickel(II) and Nickel(II)/Lanthanide(III) Chemistry
Tereza Peristeraki; Marianna Samios; Milosz Siczek; Tadeusz Lis; Constantinos J. Milios; Inorganic Chemistry 50 (2011) 5175–5185; doi:10.1021/ic2004744

data_4325281
_publ_contact_author_email       komil@chemistry.uoc.gr
_publ_contact_author_name        'Constantinos Milios'
_publ_section_title
;
 Artificial Amino Acids in Nickel(II) and Nickel(II)/Lanthanide(III)
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5175
_journal_page_last               5185
_journal_paper_doi               10.1021/ic2004744
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C26 H54 N4 Ni5 O20, 0.4(C2 H6 O1), 0.3(O H2)'
_chemical_formula_sum            'C26.8 H57 N4 Ni5 O20.7'
_chemical_formula_weight         1060.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.172(6)
_cell_length_b                   17.242(8)
_cell_length_c                   22.112(10)
_cell_measurement_reflns_used    6473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.68
_cell_volume                     5022(4)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Xcalibur PX with ONYX CCD'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.1730
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14198
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             2206
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                2700
_reflns_number_total             5484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2004744_si_001_5.cif
_cod_data_source_block           complex_4
_cod_original_formula_sum        'C26.80 H57 N4 Ni5 O20.70'
_cod_database_code               4325281