Cyclophane with Eclipsed Pyrene Units Enables Construction of Spin Interfaces with Chemical Accuracy
Metzelaars, Marvin; Schneider, Claus M.; Rawson, Jeff; Bürgler, Daniel E.; Sanz, Sergio; Matthes, Frank; Kögerler, Paul; Hattori, Takuma; Schleicher, Sebastian; Borca, Bogdana; Chemical Science  (2021) –; doi:10.1039/D1SC01036K

data_1562695
_publ_section_title
;
 Cyclophane with Eclipsed Pyrene Units Enables Construction of Spin
 Interfaces with Chemical Accuracy
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01036K
_journal_year                    2021
_chemical_formula_moiety         'C52 H32 Fe2'
_chemical_formula_sum            'C52 H32 Fe2'
_chemical_formula_weight         768.47
_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
_audit_creation_date             2020-07-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.840(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6986(3)
_cell_length_b                   10.1128(2)
_cell_length_c                   15.0273(4)
_cell_measurement_reflns_used    7035
_cell_measurement_temperature    101(3)
_cell_measurement_theta_max      28.0680
_cell_measurement_theta_min      3.3780
_cell_volume                     1620.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4623
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_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    -50.00  70.00   0.40   20.00    --  -13.90  77.00  60.00  300
  2  \w    -22.00  98.00   0.40   20.00    --   14.37  77.00 -30.00  300
  3  \w    -22.00  98.00   0.40   20.00    --   14.37  77.00  30.00  300
  4  \w    -22.00  98.00   0.40   20.00    --   14.37  77.00-180.00  300
  5  \w   -107.00 -57.00   0.40   20.00    --  -13.90-178.00  30.00  125
  6  \w   -105.00 -55.00   0.40   20.00    --  -13.90 178.00 150.00  125
  7  \w    -20.00  58.00   0.40   20.00    --   14.37 -99.00  30.00  195
  8  \w    -20.00  58.00   0.40   20.00    --   14.37 -99.00-180.00  195
  9  \w    -64.00  46.00   0.40   20.00    --   14.37 -57.00 -90.00  275
 10  \w     34.00 104.00   0.40   20.00    --   14.37-178.00  30.00  175
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067031000
_diffrn_orient_matrix_UB_12      0.0536334000
_diffrn_orient_matrix_UB_13      0.0296498000
_diffrn_orient_matrix_UB_21      -0.0518090000
_diffrn_orient_matrix_UB_22      -0.0321917000
_diffrn_orient_matrix_UB_23      0.0170775000
_diffrn_orient_matrix_UB_31      0.0412054000
_diffrn_orient_matrix_UB_32      -0.0317655000
_diffrn_orient_matrix_UB_33      0.0327408000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1170
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.296
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0447P)^2^+1.1864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             4196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01036k2.cif
_cod_data_source_block           exo_4111_abs
_cod_database_code               1562695
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              89101
_shelx_hkl_checksum              36962