Retroracemization using new forms of Belokon's original ligand: intermediate Ni^II^ complexes of <i>N</i>-({2-[<i>N</i>-(<i>S</i>)-alkylprolylamino]phenyl}phenylmethylene)-(<i>S</i>)-phenylalanine (alkyl is 2-picolyl, 3-picolyl or ethyl)
Blake, Alexander J.; De, Binod B.; Li, Wan-Sheung; Thomas, Neil R.; Acta Crystallographica Section C 58 (2002) m570–m574; doi:10.1107/S0108270102018309

data_2013090
_publ_section_title
;Retroracemization using new forms of Belokon's original ligand: intermediate
 Ni^II^ complexes of
 <i>N</i>-({2-[<i>N</i>-(<i>S</i>)-alkylprolylamino]phenyl}phenylmethylene)-(<i>S</i>)-phenylalanine
 (alkyl is 2-picolyl, 3-picolyl or ethyl)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m570
_journal_page_last               m574
_journal_paper_doi               10.1107/S0108270102018309
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni (C33 H30 N4 O3)] , 0.5H2 O'
_chemical_formula_moiety         'C33 H30 N4 Ni O3 , 0.5H2 O'
_chemical_formula_sum            'C33 H31 N4 Ni O3.5'
_chemical_formula_weight         598.33
_chemical_name_systematic
;
[N-({2-[N-(S)-(3-picolyl)prolylamino]phenyl}phenylmethylene)-(S)-
phenylalaninato]nickel(II) hemihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.522(4)
_cell_length_b                   18.623(6)
_cell_length_c                   25.828(7)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.65
_cell_measurement_theta_min      12.4
_cell_volume                     5542(3)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1995)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1995)'
_computing_molecular_graphics    'SHELXTL/PC (Bruker, 1997)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       \w/2\q
_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  0.044
_diffrn_reflns_av_sigmaI/netI    0.069
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5291
_diffrn_reflns_theta_full        23.51
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        'variation +-5.2'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1995)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details 'Flack (1983) with 194 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.29
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.29
_refine_ls_R_factor_all          0.100
_refine_ls_R_factor_gt           0.066
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+16.36P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.126
_reflns_number_gt                3785
_reflns_number_total             4765
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1578.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C33 H31 N4 Ni O3.50'
_cod_database_code               2013090
_cod_database_fobs_code          2013090