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_4325280
_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_formula_moiety         'C48 H96 N12 Ni6 O24 Pr, 3(N O3), 5.5(H2 O )'
_chemical_formula_sum            'C48 H107 N15 Ni6 O38.5 Pr'
_chemical_formula_weight         2003.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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            2
_cell_length_a                   16.373(7)
_cell_length_b                   17.206(8)
_cell_length_c                   13.912(4)
_cell_measurement_reflns_used    15539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.49
_cell_volume                     3919(3)
_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 0.969
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Xcalibur PX KM4CCD'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18237
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
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            purple
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             2070
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.51
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0285P)^2^+22.8690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                3786
_reflns_number_total             4641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2004744_si_001_4.cif
_cod_data_source_block           complex_3
_cod_original_formula_sum        'C48 H107 N15 Ni6 O38.50 Pr'
_cod_database_code               4325280