Diastereopure Fe(II) and Zn(II) Complexes Derived from a TridentateN,N‘,N-Bis(methyl-l-prolinate)-Substituted Pyridine Ligand
Gosiewska, Silvia; Cornelissen, Jeroen J. L. M.; Lutz, Martin; Spek, Anthony L.; van Koten, Gerard; Klein Gebbink, Robertus J. M.; Inorganic Chemistry 45 (2006) 4214–4227; doi:10.1021/ic060134z

data_4332229
_publ_section_title
;
 Diastereopure Fe(II) and Zn(II) Complexes Derived from a
 TridentateN,N&#x2018;,N-Bis(methyl-l-prolinate)-Substituted Pyridine
 Ligand
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4214
_journal_page_last               4227
_journal_paper_doi               10.1021/ic060134z
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H27 F6 Fe N3 O10 S2'
_chemical_formula_sum            'C21 H27 F6 Fe N3 O10 S2'
_chemical_formula_weight         715.43
_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   difmap
_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                   9.0393(6)
_cell_length_b                   13.0683(13)
_cell_length_c                   24.218(3)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.39
_cell_measurement_theta_min      3.71
_cell_volume                     2860.8(5)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35955
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0356P)^2^+0.6143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                4286
_reflns_number_total             5315
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060134zsup1.cif
_cod_data_source_block           s3045a
_cod_database_code               4332229