Design of Highly Active Iron-Based Catalysts for Atom Transfer Radical Polymerization: Tridentate Salicylaldiminato Ligands Affording near Ideal Nernstian Behavior
Rachel K. O'Reilly; Vernon C. Gibson; Andrew J. P. White; David J. Williams; Journal of the American Chemical Society 125 (2003) 8450–8451; doi:10.1021/ja035458q

data_4113909
_publ_section_title
;
 Design of Highly Active Iron-Based Catalysts for Atom Transfer Radical
 Polymerization: Tridentate Salicylaldiminato Ligands Affording near Ideal
 Nernstian Behavior
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8450
_journal_page_last               8451
_journal_paper_doi               10.1021/ja035458q
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C19 H31 Cl2 Fe N2 O'
_chemical_formula_weight         430.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.34(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.838(3)
_cell_length_b                   9.458(2)
_cell_length_c                   23.703(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      4.75
_cell_volume                     2199.2(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3218
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         3.74
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.796
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_correction_T_min  0.7822
_exptl_absorpt_correction_type   'Lamina [1 0 1]'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       needles
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00029(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_obs          0.0555
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.1800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1400
_refine_ls_wR_factor_obs         0.1163
_reflns_number_observed          2055
_reflns_number_total             2994
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035458qrom20030408_065346.cif
_cod_data_source_block           Compound4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.1800P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.1800P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2199.1(9)
_cod_original_formula_sum        'C19 H31 N2 O Cl2 Fe'
_cod_database_code               4113909