{CpFe<sup>II</sup>(CO)<sub>2</sub>Sn<sup>II</sup>(Macrocycle<sup>•3-</sup>)} Radicals with Intrinsic Charge Transfer from CpFe(CO)<sub>2</sub> to Macrocycles (Cp: Cp or Cp*); Effective Magnetic Coupling between Radical Trianionic Macrocycles<sup>•3</sup>.
Konarev, Dmitri V.; Kuzmin, Alexey V.; Batov, Mikhail S.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; ACS omega 3 (2018) 14875–14888; doi:10.1021/acsomega.8b02221

data_4516128
_publ_section_title
;
 {CpFe<sup>II</sup>(CO)<sub>2</sub>Sn<sup>II</sup>(Macrocycle<sup>&#x2022;3-</sup>)}
 Radicals with Intrinsic Charge Transfer from CpFe(CO)<sub>2</sub> to
 Macrocycles (Cp: Cp or Cp*); Effective Magnetic Coupling between Radical
 Trianionic Macrocycles<sup>&#x2022;3</sup>.
;
_journal_issue                   11
_journal_name_full               'ACS omega'
_journal_page_first              14875
_journal_page_last               14888
_journal_paper_doi               10.1021/acsomega.8b02221
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C60 H39 Fe N8 O2 Sn, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C72 H47 Cl4 Fe N8 O2 Sn'
_chemical_formula_weight         1372.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                66.775(5)
_cell_angle_beta                 86.024(5)
_cell_angle_gamma                79.263(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6681(6)
_cell_length_b                   16.5135(8)
_cell_length_c                   16.9193(10)
_cell_measurement_reflns_used    7798
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.4710
_cell_measurement_theta_min      2.2440
_cell_volume                     2943.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.896
_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     10.89 200.89   0.50   80.00    --   28.00  73.42 -25.61  380
  2  \w     10.89 200.89   0.50   80.00    --   28.00  73.42 154.39  380
  3  \w    104.39 200.39   0.50   80.00    --   28.00  73.42  94.39  192
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003130000
_diffrn_orient_matrix_UB_12      0.0443622000
_diffrn_orient_matrix_UB_13      -0.0303719000
_diffrn_orient_matrix_UB_21      -0.0130385000
_diffrn_orient_matrix_UB_22      0.0161964000
_diffrn_orient_matrix_UB_23      0.0332639000
_diffrn_orient_matrix_UB_31      0.0604835000
_diffrn_orient_matrix_UB_32      -0.0046976000
_diffrn_orient_matrix_UB_33      0.0072272000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1162
_diffrn_reflns_av_unetI/netI     0.1501
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19901
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'sealed tube'
_diffrn_source_target            MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         10784
_refine_ls_number_restraints     699
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0915
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+14.6864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1994
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6549
_reflns_number_total             10784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02221_si_002.cif
_cod_data_source_block           Comp04
_cod_database_code               4516128
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C144 H94 N16 Cl8 Fe2 O4 Sn2'
_reflns_odcompleteness_completeness 89.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 1*[Sof(Cl5)+Sof(Cl6)+Sof(C1G)+Sof(C1H)+Sof(C1I)+Sof(H1I)+Sof(C1J)+Sof(H1J)+
 Sof(C1K)+Sof(H1K)+Sof(C1L)+Sof(H1L)]+1*[Sof(Cl3)+Sof(Cl4)+Sof(C1A)+Sof(C1B)+
 Sof(C1C)+Sof(H1C)+Sof(C1D)+Sof(H1D)+Sof(C1E)+Sof(H1E)+Sof(C1F)+Sof(H1F)]+1*
 [Sof(Cl7)+Sof(Cl8)+Sof(C1M)+Sof(C1N)+Sof(C1O)+Sof(H1O)+Sof(C1P)+Sof(H1P)+
 Sof(C1Q)+Sof(H1Q)+Sof(C1R)+Sof(H1R)]=1 with esd of 0.0001
 Sof(Cl5)=Sof(Cl6)=Sof(C1G)=Sof(C1H)=Sof(C1I)=Sof(H1I)=Sof(C1J)=Sof(H1J)=
 Sof(C1K)=Sof(H1K)=Sof(C1L)=Sof(H1L)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C1A)=Sof(C1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=
 Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=FVAR(2)
 Sof(Cl7)=Sof(Cl8)=Sof(C1M)=Sof(C1N)=Sof(C1O)=Sof(H1O)=Sof(C1P)=Sof(H1P)=
 Sof(C1Q)=Sof(H1Q)=Sof(C1R)=Sof(H1R)=FVAR(3)
5.a Me refined with riding coordinates:
 C206(H20A,H20B,H20C), C207(H20D,H20E,H20F), C208(H20G,H20H,H20I), C209(H20J,
 H20K,H20L), C210(H21A,H21B,H21C)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36),
  C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
 C46(H46), C48(H48)
;
_shelx_res_checksum              69826
_shelx_hkl_checksum              20710
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.617