{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_4516127
_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         'C44 H31 Fe N8 O2 Sn, 0.5(C6 H4 Cl2)'
_chemical_formula_sum            'C47 H33 Cl Fe N8 O2 Sn'
_chemical_formula_weight         951.80
_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             2017-04-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90.491(2)
_cell_angle_beta                 91.962(2)
_cell_angle_gamma                98.758(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3737(3)
_cell_length_b                   11.6856(3)
_cell_length_c                   16.9500(4)
_cell_measurement_reflns_used    16757
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.2380
_cell_measurement_theta_min      2.0400
_cell_volume                     2029.38(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.912
_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   30.00    --   28.00  73.42 -25.61  380
  2  \w     10.89 200.89   0.50   30.00    --   28.00  73.42 154.39  380
  3  \w     10.89 200.89   0.50   30.00    --   28.00  73.42  94.39  380
  4  \w     10.89 200.89   0.50   30.00    --   28.00  73.42-145.61  380
;
_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      0.0217415000
_diffrn_orient_matrix_UB_12      0.0313086000
_diffrn_orient_matrix_UB_13      -0.0339437000
_diffrn_orient_matrix_UB_21      -0.0051334000
_diffrn_orient_matrix_UB_22      0.0527157000
_diffrn_orient_matrix_UB_23      0.0198432000
_diffrn_orient_matrix_UB_31      0.0655226000
_diffrn_orient_matrix_UB_32      0.0036472000
_diffrn_orient_matrix_UB_33      0.0144087000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.107
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'sealed tube'
_diffrn_source_target            MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9918
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0301P)^2^+2.0871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8765
_reflns_number_total             9918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02221_si_002.cif
_cod_data_source_block           Comp03
_cod_database_code               4516127
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C54H46N8O4Fe1Sn1
_reflns_odcompleteness_completeness 99.47
_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. Uiso/Uaniso restraints and constraints
C6A \\sim C7A \\sim C8A \\sim C4A \\sim C5A \\sim C9A \\sim C9 \\sim C4 \\sim
C5 \\sim C6 \\sim C8 \\sim C7: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
Cl2 \\sim Cl3 \\sim Cl2A \\sim Cl3A: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
3. Same fragment restrains
{Cl2, Cl3, C4, C5, C6, C7, C8, C9} sigma for 1-2: 0.0001, 1-3: 0.0001
as
{Cl2A, Cl3A, C4A, C5A, C6A, C7A, C8A, C9A}
4. Others
 Sof(Cl2A)=Sof(Cl3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=0.5*(1-FVAR(2))
 Sof(Cl2)=Sof(Cl3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=
 Sof(H8)=Sof(C9)=Sof(H9)=0.5*FVAR(2)
5.a Free rotating group:
 Cl2(Cl3,C4,C5,C6,C7,C8,C9)
5.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C6(H6), C7(H7), C8(H8), C9(H9),
  C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A)
5.c Idealised Me refined as rotating group:
 C206(H20A,H20B,H20C), C207(H20D,H20E,H20F), C208(H20G,H20H,H20I), C209(H20J,
 H20K,H20L), C210(H21A,H21B,H21C)
;
_shelx_res_checksum              81712
_shelx_hkl_checksum              80754
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.902