Aliphatic C-C Bond Cleavage of α-Hydroxy Ketones by Non-Heme Iron(II) Complexes: Mechanistic Insight into the Reaction Catalyzed by 2,4'-Dihydroxyacetophenone Dioxygenase.
Rahaman, Rubina; Paria, Sayantan; Paine, Tapan Kanti; Inorganic chemistry 54 (2015) 10576–10586; doi:10.1021/acs.inorgchem.5b01235

data_4344442
_publ_section_title
;
 Aliphatic C-C Bond Cleavage of \a-Hydroxy Ketones by Non-Heme Iron(II)
 Complexes: Mechanistic Insight into the Reaction Catalyzed by
 2,4'-Dihydroxyacetophenone Dioxygenase.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10576
_journal_page_last               10586
_journal_paper_doi               10.1021/acs.inorgchem.5b01235
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C51 H43 B Fe N6 O2'
_chemical_formula_sum            'C51 H43 B Fe N6 O2'
_chemical_formula_weight         838.57
_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
_audit_creation_date             2015-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.307(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4853(7)
_cell_length_b                   19.0581(9)
_cell_length_c                   16.9739(8)
_cell_measurement_reflns_used    5729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.355
_cell_measurement_theta_min      2.50
_cell_volume                     4365.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51337
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.509
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0664 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.9217. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
The unit cell contains eight disordered methanol molecule which has been treated as a diffuse 
contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON
;
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0489
_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^)+(0.1000P)^2^+0.5231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5877
_reflns_number_total             7673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01235_si_002.cif
_cod_data_source_block           rrha_sqr
_cod_depositor_comments          'Adding full bibliography for 4344442.cif.'
_cod_database_code               4344442
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C47(H47), B1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C51(H51A,H51B), C50(H50A,H50B), C49(H49A,H49B)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C19(H19), C8(H8), C11(H11), C1(H1), C5(H5), C12(H12), C15(H15),
 C14(H14), C3(H3), C4(H4), C13(H13), C2(H2), C16(H16), C23(H23), C20(H20),
 C26(H26), C30(H30), C17(H17), C18(H18), C28(H28), C27(H27), C29(H29), C45(H45),
  C41(H41), C43(H43), C38(H38), C44(H44), C42(H42), C32(H32), C35(H35),
 C33(H33), C34(H34)
;
_shelx_res_checksum              78407
_shelx_hkl_checksum              95144
_olex2_submission_special_instructions 'No special instructions were received'