Fusing pyrene and ferrocene into a chiral, redox-active triangle.
Metzelaars, Marvin; Sanz, Sergio; Rawson, Jeff; Hartmann, Rudolf; Schneider, Claus M.; Kögerler, Paul; Chemical communications (Cambridge, England) 57 (2021) 6660–6663; doi:10.1039/d1cc02191e

data_7128461
_publ_section_title
;
 Fusing pyrene and ferrocene into a chiral, redox-active triangle.
;
_journal_issue                   54
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6660
_journal_page_last               6663
_journal_paper_doi               10.1039/d1cc02191e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C42 H26 Fe'
_chemical_formula_sum            'C42 H26 Fe'
_chemical_formula_weight         586.48
_chemical_name_systematic        1,1'-Bis(2-pyrenyl)ferrocene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.87000(10)
_cell_length_b                   11.38260(10)
_cell_length_c                   22.14960(10)
_cell_measurement_reflns_used    58775
_cell_measurement_temperature    99.7(6)
_cell_measurement_theta_max      29.1780
_cell_measurement_theta_min      3.4190
_cell_volume                     5261.75(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 1.171.40.53 (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      99.7(6)
_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 0.970
_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   -105.00 -55.00   0.50   10.00    --  -13.90 178.00-120.00  100
  2  \w    -20.00  30.00   0.50   10.00    --  -13.90 -99.00-150.00  100
  3  \w    -20.00  59.00   0.50   10.00    --   14.52 -99.00 -90.00  158
  4  \w    -20.00  59.00   0.50   10.00    --   14.52 -99.00-180.00  158
  5  \w    -65.00  46.00   0.50   10.00    --   14.52 -38.00 -60.00  222
  6  \w    -65.00  46.00   0.50   10.00    --   14.52 -38.00  30.00  222
  7  \w    -20.00  30.00   0.50   10.00    --  -13.90 -99.00 120.00  100
  8  \w    -18.00  92.00   0.50   10.00    --   14.52  57.00 -30.00  220
  9  \w    -18.00  92.00   0.50   10.00    --   14.52  57.00-180.00  220
 10  \w    -20.00  26.00   0.50   10.00    --   14.52 -99.00  30.00   92
 11  \w    -22.00  99.00   0.50   10.00    --   14.52  77.00  30.00  242
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0136244000
_diffrn_orient_matrix_UB_12      -0.0523995000
_diffrn_orient_matrix_UB_13      0.0116361000
_diffrn_orient_matrix_UB_21      -0.0148932000
_diffrn_orient_matrix_UB_22      0.0326607000
_diffrn_orient_matrix_UB_23      0.0233888000
_diffrn_orient_matrix_UB_31      -0.0273410000
_diffrn_orient_matrix_UB_32      0.0083184000
_diffrn_orient_matrix_UB_33      -0.0185350000
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            110031
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.278
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78190
_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    1.481
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2432
_exptl_crystal_recrystallization_method
'grown by slow evaporation from chloroform'
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+3.5736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6418
_reflns_number_total             6970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02191e6.cif
_cod_data_source_block           exp_4118
_cod_depositor_comments
'Adding full bibliography for 7128459--7128462.cif.'
_cod_database_code               7128461
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.741
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
  C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C37(H37),
 C38(H38), C40(H40)
;
_shelx_res_checksum              14849
_shelx_hkl_checksum              30551