Redox-Tagged Carbon Monoxide-Releasing Molecules (CORMs): Ferrocene-Containing [Mn(C^N)(CO)<sub>4</sub>] Complexes as a Promising New CORM Class.
Aucott, Benjamin J.; Ward, Jonathan S.; Andrew, Samuel G.; Milani, Jessica; Whitwood, Adrian C.; Lynam, Jason M.; Parkin, Alison; Fairlamb, Ian J. S.; Inorganic chemistry 56 (2017) 5431–5440; doi:10.1021/acs.inorgchem.7b00509

data_4349434
_publ_section_title
;
 Redox-Tagged Carbon Monoxide-Releasing Molecules (CORMs):
 Ferrocene-Containing [Mn(C^N)(CO)<sub>4</sub>] Complexes as a Promising
 New CORM Class.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5431
_journal_page_last               5440
_journal_paper_doi               10.1021/acs.inorgchem.7b00509
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C21 H17 Fe N'
_chemical_formula_sum            'C21 H17 Fe N'
_chemical_formula_weight         339.21
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.974(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0034(9)
_cell_length_b                   9.3009(4)
_cell_length_c                   10.3112(5)
_cell_measurement_reflns_used    3608
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.9230
_cell_measurement_theta_min      8.1040
_cell_volume                     1515.99(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -69.00  -1.00   1.00    7.50    --    0.00 -57.00 120.00   68
  2  \w    -21.00  30.00   1.00    7.50    --    0.00  57.00-120.00   51
  3  \w     31.00  69.00   1.00    7.50    --    0.00  57.00-120.00   38
  4  \w     34.00 126.00   1.00   30.00    --   54.00  37.00-150.00   92
  5  \w     28.00 110.00   1.00   30.00    --   54.00  77.00 -90.00   82
  6  \w     -3.00  47.00   1.00   30.00    --   54.00 -57.00  90.00   50
  7  \w     38.00 111.00   1.00   30.00    --   54.00-125.00-120.00   73
  8  \w      5.00  72.00   1.00   30.00    --   54.00 -57.00 -60.00   67
  9  \w     42.00 114.00   1.00   30.00    --   54.00  57.00  60.00   72
 10  \w     36.00  92.00   1.00   30.00    --  108.00 -37.00 120.00   56
 11  \w    116.00 151.00   1.00   30.00    --  108.00 178.00 -30.00   35
 12  \w     91.00 150.00   1.00   30.00    --  108.00  77.00  60.00   59
 13  \w     40.00 102.00   1.00   30.00    --  108.00 -50.00-150.00   62
 14  \w     38.00 138.00   1.00   30.00    --  108.00 -77.00  60.00  100
 15  \w     57.00  98.00   1.00   30.00    --  108.00 178.00 -30.00   41
 16  \w     36.00  65.00   1.00   30.00    --  108.00 -37.00   0.00   29
 17  \w     45.00 105.00   1.00   30.00    --  108.00 -50.00 -60.00   60
 18  \w     47.00  90.00   1.00   30.00    --  108.00 -25.00  30.00   43
 19  \w     56.00  89.00   1.00   30.00    --  108.00 -25.00  60.00   33
 20  \w     37.00 116.00   1.00   30.00    --  108.00-111.00   0.00   79
 21  \w     38.00 111.00   1.00   30.00    --  108.00 -77.00-150.00   73
 22  \w     39.00 172.00   1.00   30.00    --  108.00  12.00  30.00  133
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0068258000
_diffrn_orient_matrix_UB_12      0.1585081000
_diffrn_orient_matrix_UB_13      0.0440292000
_diffrn_orient_matrix_UB_21      0.0970888000
_diffrn_orient_matrix_UB_22      -0.0093290000
_diffrn_orient_matrix_UB_23      0.0151577000
_diffrn_orient_matrix_UB_31      -0.0037291000
_diffrn_orient_matrix_UB_32      0.0475140000
_diffrn_orient_matrix_UB_33      -0.1439300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.578
_diffrn_reflns_theta_min         5.519
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.935
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_recrystallization_method 'chloroform evaporation'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0647P)^2^+1.6449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3456
_reflns_number_total             4139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00509_si_002.cif
_cod_data_source_block           ijsf1601_twin1_hklf4
_cod_original_cell_volume        1516.00(13)
_cod_database_code               4349434
_chemical_oxdiff_formula         'C21 H17 N Fe'
_chemical_oxdiff_usercomment     'Ben Aucott BJA-1-055'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7477(13) 0.2523(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-04
_olex2_date_sample_submission    2016-01-29
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id BJA-1-005
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.773
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.6474\% 
 around [-0.24 -0.00 0.97] (reciprocal) or [0.00 0.00 1.00] (direct)
;