Ferracyclic carbonyl complexes as anti-inflammatory agents.
Wright, Mark A.; Wooldridge, Tyler; O'Connell, Maria A; Wright, Joseph A.; Chemical communications (Cambridge, England) 56 (2020) 4300–4303; doi:10.1039/d0cc01449d

data_7126202
_publ_section_title
;
 Ferracyclic carbonyl complexes as anti-inflammatory agents.
;
_journal_issue                   31
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4300
_journal_page_last               4303
_journal_paper_doi               10.1039/d0cc01449d
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C36 H36 Fe2 N4 O16 S2, 3(C H4 O), 1.5(H2 O)'
_chemical_formula_sum            'C39 H51 Fe2 N4 O20.5 S2'
_chemical_formula_weight         1079.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-09 deposited with the CCDC.	2020-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.705(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8608(7)
_cell_length_b                   13.3771(5)
_cell_length_c                   15.4092(5)
_cell_measurement_reflns_used    14750
_cell_measurement_temperature    139.9(8)
_cell_measurement_theta_max      28.7110
_cell_measurement_theta_min      3.2970
_cell_volume                     4816.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.9(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details
;
  1 omega   -1.00   85.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -       16.5972   57.0000  -90.0000 86

  2 omega  -13.00   87.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -       16.5972   77.0000   60.0000 100

  3 omega  -25.00   58.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -       16.5972  -99.0000  120.0000 83

  4 omega    1.00   85.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -       16.5972   57.0000 -180.0000 84

  5 omega   -1.00   78.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -       16.5972   38.0000    0.0000 79

  6 omega  -50.00   49.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -      -20.0347   77.0000 -180.0000 99

  7 omega  -40.00   49.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -      -20.0347   57.0000  -60.0000 89

  8 omega  -21.00   49.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -      -20.0347   57.0000   30.0000 70

  9 omega  -78.00   -7.00   1.0000   22.8900
omega____ theta____ kappa____ phi______ frames
    -      -20.0347  126.0000  -63.4732 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0395725000
_diffrn_orient_matrix_UB_12      -0.0284700000
_diffrn_orient_matrix_UB_13      -0.0034281000
_diffrn_orient_matrix_UB_21      0.0239184000
_diffrn_orient_matrix_UB_22      -0.0398496000
_diffrn_orient_matrix_UB_23      0.0156135000
_diffrn_orient_matrix_UB_31      -0.0085070000
_diffrn_orient_matrix_UB_32      0.0203317000
_diffrn_orient_matrix_UB_33      0.0258050000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36750
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.305
_diffrn_reflns_theta_min         3.090
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       prism
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.684
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.02(3)
_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     644
_refine_ls_number_reflns         11488
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+8.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                8304
_reflns_number_total             11488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01449d2.cif
_cod_data_source_block           matts1
_cod_depositor_comments
'Adding full bibliography for 7126201--7126202.cif.'
_cod_original_formula_sum        'C39 H51 Fe2 N4 O20.50 S2'
_cod_database_code               7126202
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H30N2Au
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.759
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.02(3)
 -0.02(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 O21-C39 = O21A-C39A
 1.445 with sigma of 0.005
 H4-H13a
 3.5 with sigma of 0.04
 H19a-H18
 1.85 with sigma of 0.04
 H19b-H4
 1.85 with sigma of 0.04
 H7A-H16
 1.99 with sigma of 0.04
 C39A-O21A \\sim C39-O21
 with sigma of 0.02
 O7-C18 \\sim O7A-C18
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C39A) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O21) = Uanis(O21A)
Uanis(C39) = Uanis(C39A)
Uanis(O7) = Uanis(O7A)
5. Others
 Sof(O21A)=Sof(H21A)=Sof(C39A)=Sof(H39d)=Sof(H39e)=Sof(H39f)=1-FVAR(1)
 Sof(O21)=Sof(H21)=Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(H39c)=FVAR(1)
 Sof(O7A)=Sof(H7A)=Sof(H18c)=Sof(H18d)=1-FVAR(2)
 Sof(O7)=Sof(H7)=Sof(H18a)=Sof(H18b)=FVAR(2)
 Fixed Sof: H20a(0.5) H20b(0.5)
6.a Free rotating group:
 O19(H19a,H19b), O20(H20a,H20b)
6.b Ternary CH refined with riding coordinates:
 C13(H13a), C14(H14a), C15(H15a), C16(H16), C17(H17), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
6.c Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C18(H18c,H18d), C36(H36a,H36b)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4a), C1(H1), C2(H2a), C4(H4b), C5(H5a), C6(H6a), C7(H7b),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
6.e Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C39A(H39d,H39e,
 H39f)
6.f Idealised tetrahedral OH refined as rotating group:
 O4(H4), O5(H5), O6(H6), O7(H7), O7A(H7A), O12(H12), O13(H13), O14(H14),
 O15(H15), O17(H17a), O18(H18), O21(H21), O21A(H21A)
;
_shelx_res_checksum              88444
_olex2_submission_special_instructions 'No special instructions were received'