Synthesis and reactivity of a 4His enzyme model complex
Li, Jia; Banerjee, Atanu; Hasse, Timothy A.; Loloee, Reza; Biros, Shannon M.; Staples, Richard J.; Chavez, Ferman A.; RSC Adv. 7 (2017) 50713–; doi:10.1039/C7RA09456F

data_7229458
_publ_section_title
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 Synthesis and reactivity of a 4His enzyme model complex
;
_journal_issue                   80
_journal_name_full               'RSC Adv.'
_journal_page_first              50713
_journal_paper_doi               10.1039/C7RA09456F
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C90 H72 F6 Fe N8 O6 S2, 2(C4 H10 O)'
_chemical_formula_sum            'C98 H92 F6 Fe N8 O8 S2'
_chemical_formula_weight         1743.76
_chemical_name_systematic        '[Fe(TrIm)4(OTf)2]'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                98.0060(10)
_cell_angle_beta                 116.1990(10)
_cell_angle_gamma                93.3490(10)
_cell_formula_units_Z            1
_cell_length_a                   13.2342(7)
_cell_length_b                   13.5131(7)
_cell_length_c                   13.7025(7)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.355
_cell_measurement_theta_min      2.304
_cell_volume                     2157.4(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         1.536
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0505 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9392.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         7927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0489P)^2^+0.9459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6361
_reflns_number_total             7927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09456f2.cif
_cod_data_source_block           cf316a_0m_a
_cod_original_cell_volume        2157.39(19)
_cod_database_code               7229458
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C1A(H1A), C2A(H2A), C3A(H3A), C6A(H6A), C7A(H7A), C8A(H8A),
 C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A),
 C16A(H16A), C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A)
2.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_olex2_submission_special_instructions 'No special instructions were received'