Diiron(ii) pentacarbonyl complexes as CO-releasing molecules: their synthesis, characterization, CO-releasing behaviour and biocompatibility.
Xiao, Zhiyin; Jiang, Ran; Jin, Jing; Yang, Xiuqin; Xu, Binyu; Liu, Xiaoming; He, Yabing; He, Yi; Dalton transactions (Cambridge, England : 2003) 48 (2019) 468–477; doi:10.1039/c8dt03982h

data_7048282
_publ_section_title
;
 Diiron(ii) pentacarbonyl complexes as CO-releasing molecules: their
 synthesis, characterization, CO-releasing behaviour and biocompatibility.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              468
_journal_page_last               477
_journal_paper_doi               10.1039/c8dt03982h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 H21 Br Fe2 O5 S3'
_chemical_formula_sum            'C14 H21 Br Fe2 O5 S3'
_chemical_formula_weight         557.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-01-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5433)
;
_audit_update_record
;
2018-06-12 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.389(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6484(3)
_cell_length_b                   14.9685(6)
_cell_length_c                   17.1875(6)
_cell_measurement_reflns_used    4262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.5910
_cell_measurement_theta_min      3.9310
_cell_volume                     2201.18(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.967
_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     44.00 104.00   1.00    7.95    --   36.58  77.00 -30.00   60
  2  \w    -31.00  22.00   1.00    7.95    --   36.58 -77.00-150.00   53
  3  \w     53.00 109.00   1.00    7.95    --   36.58-178.00-120.00   56
  4  \w     20.00  72.00   1.00    7.95    --   36.58 -99.00 -60.00   52
  5  \w     -3.00  71.00   1.00    7.95    --   36.58 -99.00  60.00   74
  6  \w     49.00 106.00   1.00    7.95    --   36.58  38.00 -90.00   57
  7  \w     52.00  91.00   1.00    7.95    --   36.58  57.00  60.00   39
  8  \w     32.00  76.00   1.00    7.95    --   36.58 -99.00-150.00   44
  9  \w    -33.00  38.00   1.00    7.95    --   36.58 -38.00  90.00   71
 10  \w    -32.00  29.00   1.00    7.95    --   36.58 -38.00 -60.00   61
 11  \w     64.00 105.00   1.00   31.81    --  108.00-111.00-120.00   41
 12  \w     40.00 125.00   1.00   31.81    --  108.00 -45.00 -30.00   85
 13  \w    147.00 175.00   1.00   31.81    --  108.00  77.00 -60.00   28
 14  \w     40.00 125.00   1.00   31.81    --  108.00 -45.00-120.00   85
 15  \w     42.00 122.00   1.00   31.81    --  108.00 -45.00 150.00   80
 16  \w    104.00 131.00   1.00   31.81    --  108.00 -77.00  60.00   27
 17  \w     92.00 129.00   1.00   31.81    --  108.00  45.00 120.00   37
 18  \w     57.00  84.00   1.00   31.81    --  108.00 -77.00  60.00   27
 19  \w     47.00 110.00   1.00   31.81    --  108.00 -95.00 -90.00   63
 20  \w    104.00 153.00   1.00   31.81    --  108.00 111.00 -90.00   49
 21  \w     90.00 177.00   1.00   31.81    --  108.00  30.00 -30.00   87
 22  \w     50.00 110.00   1.00   31.81    --  108.00 -95.00   0.00   60
 23  \w     63.00 170.00   1.00   31.81    --  108.00   0.00  90.00  107
 24  \w     47.00 115.00   1.00   31.81    --  108.00-111.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1615966000
_diffrn_orient_matrix_UB_12      -0.0080848000
_diffrn_orient_matrix_UB_13      0.0268670000
_diffrn_orient_matrix_UB_21      0.0498367000
_diffrn_orient_matrix_UB_22      -0.0891963000
_diffrn_orient_matrix_UB_23      0.0410209000
_diffrn_orient_matrix_UB_31      0.0615267000
_diffrn_orient_matrix_UB_32      0.0508613000
_diffrn_orient_matrix_UB_33      0.0761808000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11999
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.239
_diffrn_reflns_theta_min         3.934
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       sheets
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.590
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.2354
_refine_ls_R_factor_gt           0.1705
_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^)+(0.1700P)^2^+118.0505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4141
_refine_ls_wR_factor_ref         0.4658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2706
_reflns_number_total             4206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03982h2.cif
_cod_data_source_block           4Br
_cod_depositor_comments
'Adding full bibliography for 7048280--7048283.cif.'
_cod_database_code               7048282
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe, S, C, H, Br, O'
_reflns_odcompleteness_completeness 98.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C8
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C1, O1
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
4. Uiso/Uaniso restraints and constraints
C1 \\sim O1: within 2A with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C13(H13A,H13B)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.544
_oxdiff_exptl_absorpt_empirical_full_min 0.457