{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_4516130
_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         'C39 H21 Fe In N8 O2'
_chemical_formula_sum            'C39 H21 Fe In N8 O2'
_chemical_formula_weight         804.31
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.033(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9770(2)
_cell_length_b                   21.1365(2)
_cell_length_c                   11.0927(1)
_cell_measurement_reflns_used    21241
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5980
_cell_measurement_theta_min      2.4220
_cell_volume                     3164.91(6)
_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      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_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     35.00 110.00   1.00   40.00    --   20.14 178.00-180.00   75
  2  \w    -12.00  19.00   1.00   40.00    --  -20.30 -99.00 -60.00   31
  3  \w     29.00  54.00   1.00   40.00    --  -20.30  57.00 -60.00   25
  4  \w    -83.00  -8.00   1.00   40.00    --  -20.30 -57.00 -30.00   75
  5  \w    -52.00  58.00   1.00   40.00    --  -20.30  77.00 -90.00  110
  6  \w    -54.00  47.00   1.00   40.00    --  -20.30  77.00-180.00  101
;
_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      0.0369986000
_diffrn_orient_matrix_UB_12      -0.0229315000
_diffrn_orient_matrix_UB_13      0.0245083000
_diffrn_orient_matrix_UB_21      0.0086104000
_diffrn_orient_matrix_UB_22      -0.0036800000
_diffrn_orient_matrix_UB_23      -0.0598370000
_diffrn_orient_matrix_UB_31      0.0363288000
_diffrn_orient_matrix_UB_32      0.0242368000
_diffrn_orient_matrix_UB_33      0.0140888000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.823
_diffrn_reflns_theta_min         1.790
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.810
_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    1.688
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.7189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9496
_reflns_number_total             10910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02221_si_002.cif
_cod_data_source_block           Comp06
_cod_database_code               4516130
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C39 H21 Fe1 In1 O2 N8'
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.758
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105), C106(H106), C111(H111), C112(H112),
 C113(H113), C114(H114), C119(H119), C120(H120), C121(H121), C122(H122),
 C127(H127), C128(H128), C129(H129), C130(H130), C201(H201), C202(H202),
 C203(H203), C204(H204), C205(H205)
;
_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 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.914