{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_4516129
_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         'C51 H33 Fe N4 O2 Sn'
_chemical_formula_sum            'C51 H33 Fe N4 O2 Sn'
_chemical_formula_weight         908.35
_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             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90.824(3)
_cell_angle_beta                 91.078(3)
_cell_angle_gamma                97.186(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2634(4)
_cell_length_b                   11.3120(4)
_cell_length_c                   14.9929(5)
_cell_measurement_reflns_used    12837
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      29.4050
_cell_measurement_theta_min      2.7620
_cell_volume                     1894.66(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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_environment      N~2~
_diffrn_ambient_temperature      111(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.894
_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     43.00 101.00   1.00   64.00    --   12.05 178.00 -30.00   58
  2  \w    -39.00  31.00   1.00   64.00    --  -12.36  37.00   0.00   70
  3  \w    -25.00  30.00   1.00   64.00    --  -12.36 -99.00  90.00   55
  4  \w    -97.00 -70.00   1.00   64.00    --  -12.36-178.00-150.00   27
  5  \w    -81.00 -51.00   1.00   64.00    --  -12.36 -37.00  90.00   30
  6  \w    -22.00   9.00   1.00   64.00    --  -12.36 -37.00  90.00   31
  7  \w    -89.00  14.00   1.00   64.00    --  -12.36 -37.00   0.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0523972000
_diffrn_orient_matrix_UB_12      0.0391860000
_diffrn_orient_matrix_UB_13      0.0115227000
_diffrn_orient_matrix_UB_21      0.0068703000
_diffrn_orient_matrix_UB_22      -0.0321205000
_diffrn_orient_matrix_UB_23      0.0396673000
_diffrn_orient_matrix_UB_31      0.0352062000
_diffrn_orient_matrix_UB_32      -0.0377686000
_diffrn_orient_matrix_UB_33      -0.0230939000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       irregular
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.497
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         8958
_refine_ls_number_restraints     356
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0405P)^2^+1.5666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8716
_reflns_number_total             8958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02221_si_002.cif
_cod_data_source_block           Comp05
_cod_database_code               4516129
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C51H33N4O2Fe1Sn1
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6241(8)
 0.3759(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C301 \\sim C302 \\sim
C303 \\sim C304 \\sim C305: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim
C146 \\sim C147 \\sim C148 \\sim C149 \\sim C150: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq, Uanis(C303) \\sim Ueq,
Uanis(C304) \\sim Ueq, Uanis(C305) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C141) \\sim Ueq,
Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Fe3) = Uanis(Fe2)
Uanis(C207) = Uanis(C307)
Uanis(C206) = Uanis(C306)
Uanis(O207) = Uanis(O307)
Uanis(O206) = Uanis(O306)
4. Same fragment restrains
{Fe2, O206, O207, C201, C202, C203, C204, C205, C206, C207} sigma for 1-2:
0.001, 1-3: 0.001
as
{Fe3, O306, O307, C301, C302, C303, C304, C305, C306, C307}
{C139, C140, C141, C142, C143, C144} sigma for 1-2: 0.001, 1-3: 0.001
as
{C145, C146, C147, C148, C149, C150}
5. Others
 Sof(Fe3)=Sof(O306)=Sof(O307)=Sof(C301)=Sof(H301)=Sof(C302)=Sof(H302)=
 Sof(C303)=Sof(H303)=Sof(C304)=Sof(H304)=Sof(C305)=Sof(H305)=Sof(C306)=
 Sof(C307)=1-FVAR(1)
 Sof(Fe2)=Sof(O206)=Sof(O207)=Sof(C201)=Sof(H201)=Sof(C202)=Sof(H202)=
 Sof(C203)=Sof(H203)=Sof(C204)=Sof(H204)=Sof(C205)=Sof(H205)=Sof(C206)=
 Sof(C207)=FVAR(1)
 Sof(C145)=Sof(C146)=Sof(H146)=Sof(C147)=Sof(H147)=Sof(C148)=Sof(H148)=
 Sof(C149)=Sof(H149)=Sof(C150)=Sof(H150)=1-FVAR(2)
 Sof(C139)=Sof(C140)=Sof(H140)=Sof(C141)=Sof(H141)=Sof(C142)=Sof(H142)=
 Sof(C143)=Sof(H143)=Sof(C144)=Sof(H144)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C108(H108), C109(H109), C113(H113), C114(H114),
 C118(H118), C119(H119), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C201(H201),
 C202(H202), C203(H203), C204(H204), C205(H205), C140(H140), C141(H141),
 C142(H142), C143(H143), C144(H144), C301(H301), C302(H302), C303(H303),
 C304(H304), C305(H305), C146(H146), C147(H147), C148(H148), C149(H149),
 C150(H150)
;
_shelx_res_checksum              48329
_shelx_hkl_checksum              69826
_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 1.048
_oxdiff_exptl_absorpt_empirical_full_min 0.926