A water-soluble iron-porphyrin complex capable of rescuing CO-poisoned red blood cells
Droege, Daniel G.; Johnstone, Timothy C.; Chemical Communications  (2022) –; doi:10.1039/D1CC05542A

data_7129663
_publ_section_title
;
 A water-soluble iron-porphyrin complex capable of rescuing CO-poisoned
 red blood cells
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05542A
_journal_year                    2022
_chemical_formula_moiety         'C104 H93 Fe N4 O Si4, C2 H3 N, C H2 Cl2'
_chemical_formula_sum            'C107 H98 Cl2 Fe N5 O Si4'
_chemical_formula_weight         1709.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-10 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3187(2)
_cell_length_b                   12.8480(2)
_cell_length_c                   23.5087(2)
_cell_measurement_reflns_used    34926
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7440
_cell_measurement_theta_min      2.7930
_cell_volume                     4718.53(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -51.00  21.00   0.50    0.42    --  -49.41  48.00-154.00  144
  2  \w   -121.00 -48.00   0.50    0.42    --  -49.41 -48.00  57.00  146
  3  \w    -15.00  44.00   0.50    0.42    --   49.41 -48.00  57.00  118
  4  \w     53.00  82.00   0.50    0.42    --   49.41  48.00-154.00   58
  5  \w   -115.00 -90.00   0.50    1.68    --  -84.25 -48.00  57.00   50
  6  \w    -52.00 -24.00   0.50    1.68    --  -84.25  48.00-154.00   56
  7  \w    121.00 153.00   0.50    1.68    --  105.75  48.00-154.00   64
  8  \w    -25.00  11.00   0.50    0.42    --  -49.41  19.00-120.00   72
  9  \w   -114.00 -87.00   0.50    0.42    --  -49.41 -57.00   0.00   54
 10  \w   -120.00 -94.00   0.50    0.42    --  -49.41-125.00 -30.00   52
 11  \w   -121.00 -90.00   0.50    0.42    --  -49.41-125.00  30.00   62
 12  \w   -114.00 -82.00   0.50    0.42    --  -49.41 -57.00 120.00   64
 13  \w   -119.00 -94.00   0.50    0.42    --  -49.41-125.00-150.00   50
 14  \w     43.00  75.00   0.50    0.42    --   49.41  38.00 -60.00   64
 15  \w     46.00  75.00   0.50    0.42    --   49.41  38.00 -30.00   58
 16  \w     83.00 108.00   0.50    0.42    --   49.41  57.00   0.00   50
 17  \w   -107.00 -75.00   0.50    1.68    --  -84.25 -54.00 -97.03   64
 18  \w    -98.00 -72.00   0.50    1.68    --  -84.25 -55.00 -62.96   52
 19  \w    -99.00 -74.00   0.50    1.68    --  -84.25 -50.00 -29.72   50
 20  \w    -63.00 -37.00   0.50    1.68    --  -84.25  57.00 120.00   52
 21  \w    -97.00 -72.00   0.50    1.68    --  -84.25 -54.00 -39.94   50
 22  \w    -41.00 -14.00   0.50    1.68    --  -84.25  38.00  60.00   54
 23  \w    -98.00 -73.00   0.50    1.68    --  -84.25 -51.00 -55.27   50
 24  \w   -103.00 -77.00   0.50    1.68    --  -84.25 -56.00 -77.55   52
 25  \w   -132.00-107.00   0.50    1.68    --  -84.25 -56.00 -65.92   50
 26  \w   -153.00 -76.00   0.50    1.68    --  -84.25 -56.00 -99.26  154
 27  \w   -143.00-117.00   0.50    1.68    --  -84.25 -51.00 -55.27   52
 28  \w    -98.00 -73.00   0.50    1.68    --  -84.25 -55.00 -52.97   50
 29  \w   -156.00-131.00   0.50    1.68    --  -84.25 -55.00 -62.96   50
 30  \w   -155.00-101.00   0.50    1.68    --  -84.25 -77.00 150.00  108
 31  \w   -101.00 -76.00   0.50    1.68    --  -84.25 -56.00 -65.92   50
 32  \w   -139.00 -79.00   0.50    1.68    --  -84.25 -38.00   0.00  120
 33  \w     43.00  92.00   0.50    1.68    --  105.75 -77.00  30.00   98
 34  \w     96.00 174.00   0.50    1.68    --  105.75  57.00 -60.00  156
 35  \w     35.00  67.00   0.50    1.68    --  105.75 -57.00 -90.00   64
 36  \w     34.00  65.00   0.50    1.68    --  105.75 -57.00 -60.00   62
 37  \w    150.00 178.00   0.50    1.68    --  105.75 125.00  60.00   56
 38  \w    106.00 140.00   0.50    1.68    --  105.75 125.00  60.00   68
 39  \w     40.00  65.00   0.50    1.68    --  105.75 -57.00 150.00   50
 40  \w    140.00 177.00   0.50    1.68    --  105.75  57.00 -30.00   74
 41  \w     97.00 136.00   0.50    1.68    --  105.75  57.00 -30.00   78
 42  \w     98.00 175.00   0.50    1.68    --  105.75  38.00 -90.00  154
 43  \w     35.00  67.00   0.50    1.68    --  105.75 -57.00  30.00   64
 44  \w     35.00  62.00   0.50    1.68    --  105.75 -57.00  90.00   54
 45  \w     36.00  66.00   0.50    1.68    --  105.75 -57.00 -30.00   60
 46  \w     86.00 111.00   0.50    1.68    --  105.75-125.00-180.00   50
 47  \w    134.00 160.00   0.50    1.68    --  105.75  19.00   0.00   52
 48  \w     35.00  71.00   0.50    1.68    --  105.75-125.00-180.00   72
 49  \w     54.00  80.00   0.50    1.68    --  105.75 -77.00-150.00   52
 50  \w    101.00 127.00   0.50    1.68    --  105.75  19.00   0.00   52
 51  \w     34.00  59.00   0.50    1.68    --  105.75 -57.00  60.00   50
 52  \w    102.00 131.00   0.50    1.68    --  105.75  77.00  30.00   58
 53  \w    153.00 178.00   0.50    1.68    --  105.75  77.00  30.00   50
 54  \w     93.00 175.00   0.50    1.68    --  105.75  57.00   0.00  164
 55  \w    151.00 178.00   0.50    1.68    --  105.75  19.00 150.00   54
 56  \w     37.00  66.00   0.50    1.68    --  105.75 -57.00-180.00   58
 57  \w     63.00 104.00   0.50    1.68    --  105.75 -99.00 150.00   82
 58  \w     98.00 133.00   0.50    1.68    --  105.75  19.00 150.00   70
 59  \w     93.00 140.00   0.50    1.68    --  105.75  57.00 -90.00   94
 60  \w     48.00  74.00   0.50    1.68    --  105.75 -77.00 -90.00   52
 61  \w     37.00  73.00   0.50    1.68    --  105.75 -77.00  90.00   72
 62  \w     42.00  67.00   0.50    1.68    --  105.75 -57.00 120.00   50
 63  \w     35.00  66.00   0.50    1.68    --  105.75 -57.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0870392000
_diffrn_orient_matrix_UB_12      -0.0475474000
_diffrn_orient_matrix_UB_13      -0.0008765000
_diffrn_orient_matrix_UB_21      -0.0418452000
_diffrn_orient_matrix_UB_22      0.0528814000
_diffrn_orient_matrix_UB_23      -0.0602264000
_diffrn_orient_matrix_UB_31      0.0198746000
_diffrn_orient_matrix_UB_32      -0.0965672000
_diffrn_orient_matrix_UB_33      -0.0325182000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         2.829
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0868P)^2^+5.3675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7681
_reflns_number_total             8417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05542a2.cif
_cod_data_source_block           5
_cod_database_code               7129663
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C107 H98 Fe N5 Si4 O Cl2'
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.491
_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, All O(H) groups
2. Others
 Fixed Sof: Fe01(0.25) Fe02(0.25) O1A(0.25) H1A(0.25) O1B(0.25) H1B(0.25)
 Cl2(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) N3SA(0.25) C1SA(0.25) H1SA(0.25)
 H1SB(0.25) H1SC(0.25) C2SA(0.25) N3SB(0.25) C1SB(0.25) H1SD(0.25) H1SE(0.25)
 H1SF(0.25) C2SB(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C13(H13), C15(H15), C63(H63), C65(H65),
 C122(H122), C123(H123), C124(H124), C125(H125), C126(H126), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C622(H622), C623(H623),
 C624(H624), C625(H625), C626(H626), C662(H662), C663(H663), C664(H664),
 C665(H665), C666(H666)
3.c Tetrahedral OH refined as rotating group:
 O1A(H1A), O1B(H1B)
3.d Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C1SA(H1SA,H1SB,H1SC),
 C1SB(H1SD,H1SE,H1SF)
;
_shelx_res_checksum              42380
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.633
_oxdiff_exptl_absorpt_empirical_full_min 0.823