Redox-Controlled Polymerization of Lactide Catalyzed by Bis(imino)pyridine Iron Bis(alkoxide) Complexes
Ashley B. Biernesser; Bo Li; Jeffery A. Byers; Journal of the American Chemical Society 135 (2013) 16553–16560; doi:10.1021/ja407920d

data_4121084
_publ_section_title
;
 Redox-Controlled Polymerization of Lactide Catalyzed by
 Bis(imino)pyridine Iron Bis(alkoxide) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16553
_journal_page_last               16560
_journal_paper_doi               10.1021/ja407920d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C39 H41 Fe N3 O4, F6 P, C6 H6'
_chemical_formula_sum            'C45 H47 F6 Fe N3 O4 P'
_chemical_formula_weight         894.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.859(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1694(15)
_cell_length_b                   11.6266(9)
_cell_length_c                   15.5172(9)
_cell_measurement_reflns_used    4112
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      3.75
_cell_volume                     4251.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker Kappa DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1156
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23734
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.381
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\uS'
_exptl_absorpt_coefficient_mu    3.828
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2008). SADABS v2008/1. Bruker AXS Inc. Madison, WI USA.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7213
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0571P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4842
_reflns_number_total             7213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja407920d_si_001.cif
_cod_data_source_block           C45H47F6FeN3O4P
_cod_database_code               4121084
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-2
_shelx_res_checksum              63590