Dehydrogenative α-Oxygenation of Ethers with an Iron Catalyst.
Gonzalez-de-Castro, Angela; Robertson, Craig M.; Xiao, Jianliang; Journal of the American Chemical Society 136 (2014) 8350–8360; doi:10.1021/ja502167h

data_4121912
_publ_section_title
;
 Dehydrogenative \a-Oxygenation of Ethers with an Iron Catalyst.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8350
_journal_page_last               8360
_journal_paper_doi               10.1021/ja502167h
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C61 H67 F6 Fe N5 O11 S4'
_chemical_formula_sum            'C61 H67 F6 Fe N5 O11 S4'
_chemical_formula_weight         1344.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9840(8)
_cell_length_b                   10.9840(8)
_cell_length_c                   52.464(4)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.19
_cell_volume                     6329.7(8)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            79786
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6501
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+5.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                6306
_reflns_number_total             6501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja502167h_si_001.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 4121911--4121914.cif.'
_cod_database_code               4121912
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.064) H2A(0.126) H2B(0.126) H2C(0.126) H10(0.032) H12(0.039)
 H14(0.022) H16(0.037) H17(0.029) H18(0.024) H20(0.027) H23(0.041) H24(0.021)
 H27(0.028) H29(0.038) H30(0.036) H31A(0.053) H31B(0.053) H32(0.036) H33(0.039)
 H34(0.062) H35(0.053) H39A(0.088) H39B(0.088) H39C(0.088) H40(0.052)
 H42A(0.083) H42B(0.083) H42C(0.083) H44(0.078) H48A(0.051) H48B(0.051)
 H51(0.092) H52(0.047)
 Fixed X: H1(0.9574) H2A(0.6772) H2B(0.556) H2C(0.6123) H10(0.4691)
 H12(0.1077) H14(0.6016) H16(0.1133) H17(0.2967) H18(0.5707) H20(0.7519)
 H23(0.6543) H24(0.5079) H27(0.6182) H29(0.2853) H30(0.7661) H31A(0.2052)
 H31B(0.3299) H32(0.6836) H33(0.5777) H34(0.4771) H35(0.6359) H39A(0.4273)
 H39B(0.3632) H39C(0.3604) H40(0.8646) H42A(0.4445) H42B(0.4452) H42C(0.5646)
 H44(0.4322) H48A(0.2868) H48B(0.363) H51(0.3735) H52(0.6887)
 Fixed Y: H1(0.9574) H2A(0.2692) H2B(0.1958) H2C(0.2112) H10(0.5541)
 H12(0.5286) H14(0.5648) H16(0.6849) H17(0.7729) H18(0.7533) H20(0.8354)
 H23(0.3448) H24(0.788) H27(0.7885) H29(0.4639) H30(0.4801) H31A(0.328)
 H31B(0.2748) H32(0.7472) H33(0.6078) H34(1.2527) H35(1.1915) H39A(0.3144)
 H39B(0.2791) H39C(0.4143) H40(0.9002) H42A(0.491) H42B(0.359) H42C(0.4371)
 H44(0.9084) H48A(0.5155) H48B(0.4774) H51(1.1098) H52(0.9893)
 Fixed Z: H1(0) H2A(-0.1681) H2B(-0.1717) H2C(-0.1444) H10(-0.0856) H12(-
 0.0766) H14(-0.0509) H16(-0.0476) H17(-0.0362) H18(-0.09) H20(-0.0623) H23(-
 0.1133) H24(-0.0383) H27(0.0487) H29(-0.0962) H30(-0.0894) H31A(0.0158)
 H31B(0.0261) H32(-0.139) H33(-0.1637) H34(-0.0785) H35(-0.0531) H39A(-0.1254)
 H39B(-0.1511) H39C(-0.1415) H40(0.0382) H42A(-0.1809) H42B(-0.1922) H42C(-
 0.1924) H44(-0.1012) H48A(0.0086) H48B(0.0328) H51(-0.1015) H52(-0.0507) C1(0)
 N4(0) O3(0) Fe1(0)
;