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_7048280
_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         'C11 H15 Br Fe2 O5 S3'
_chemical_formula_sum            'C11 H15 Br Fe2 O5 S3'
_chemical_formula_weight         515.02
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-12
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-12 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.111(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0887(12)
_cell_length_b                   15.4561(7)
_cell_length_c                   16.3446(15)
_cell_measurement_reflns_used    3724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.2330
_cell_measurement_theta_min      2.9200
_cell_volume                     3863.0(5)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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 0.999
_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    -24.00  23.00   1.00  120.00    --  -15.58 -99.00 120.00   47
  2  \w    -24.00   3.00   1.00  120.00    --  -15.58 -99.00-150.00   27
  3  \w     23.00  87.00   1.00  120.00    --   15.89  19.00-120.00   64
  4  \w    -22.00  55.00   1.00  120.00    --   15.89 -99.00 -60.00   77
  5  \w    -50.00  33.00   1.00  120.00    --   15.89 -57.00 -30.00   83
  6  \w     17.00  43.00   1.00  120.00    --   15.89  57.00-180.00   26
  7  \w     55.00  82.00   1.00  120.00    --   15.89  19.00 -90.00   27
  8  \w     -3.00  85.00   1.00  120.00    --   15.89  38.00 120.00   88
;
_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      -0.0440691000
_diffrn_orient_matrix_UB_12      0.0104306000
_diffrn_orient_matrix_UB_13      -0.0041786000
_diffrn_orient_matrix_UB_21      -0.0071864000
_diffrn_orient_matrix_UB_22      0.0113798000
_diffrn_orient_matrix_UB_23      -0.0436837000
_diffrn_orient_matrix_UB_31      -0.0125233000
_diffrn_orient_matrix_UB_32      -0.0432300000
_diffrn_orient_matrix_UB_33      -0.0125252000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.1955
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33263
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74241
_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            dark-red
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7999
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.2120
_refine_ls_R_factor_gt           0.0840
_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^)+(0.0860P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3112
_reflns_number_total             7999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03982h2.cif
_cod_data_source_block           JR171125-Fe2Et3Br
_cod_depositor_comments
'Adding full bibliography for 7048280--7048283.cif.'
_cod_database_code               7048280
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe C O S H Br'
_shelx_estimated_absorpt_t_max   0.442
_shelx_estimated_absorpt_t_min   0.368
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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-O7
 0.99 with sigma of 0.01
 C13-C14
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              15191
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.780