Fast, solvent-free synthesis of ferrocene-containing organic cages <i>via</i> dynamic covalent chemistry in the solid state.
Kunde, Tom; Pausch, Tobias; Guńka, Piotr A; Krzyżanowski, Maurycy; Kasprzak, Artur; Schmidt, Bernd M.; Chemical science 13 (2022) 2877–2883; doi:10.1039/d1sc06372c

data_1566274
_publ_section_title
;
 Fast, solvent-free synthesis of ferrocene-containing organic cages
 <i>via</i> dynamic covalent chemistry in the solid state.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2877
_journal_page_last               2883
_journal_paper_doi               10.1039/d1sc06372c
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H18 Fe O2'
_chemical_formula_sum            'C24 H18 Fe O2'
_chemical_formula_weight         394.254
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_Int_Tables_number      43
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c4697 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-10-25 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3424(2)
_cell_length_b                   25.8718(6)
_cell_length_c                   11.9601(3)
_cell_measurement_reflns_used    17482
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.4630
_cell_measurement_theta_min      4.6140
_cell_volume                     3509.67(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9759
_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 -101.00 -38.00 0.50 17.00 -- -11.24-179.00 -90.00 126
 2 \w 1.00 54.00 0.50 17.00 -- 11.71 -99.00-120.00 106
 3 \w -70.00 58.00 0.50 17.00 -- 11.71 -19.00 90.00 256
 4 \w -87.00 15.00 0.50 17.00 -- -11.24 -38.00 150.00 204
 5 \w -18.00 45.00 0.50 17.00 -- 11.71 -77.00 -60.00 126
 6 \w -18.00 86.00 0.50 17.00 -- 11.71 57.00 120.00 208
 7 \w -22.00 39.00 0.50 17.00 -- 11.71 77.00 30.00 122
 8 \w 25.00 72.00 0.50 17.00 -- 11.71-130.00 143.00 94
 9 \w -22.00 39.00 0.50 17.00 -- 11.71 77.00-120.00 122
 10 \w -86.00 16.00 0.50 17.00 -- -11.24 -42.00 10.00 204
 11 \w -45.00 39.00 0.50 17.00 -- -11.24 77.00 -30.00 168
 12 \w -22.00 39.00 0.50 17.00 -- 11.71 77.00 -30.00 122
 13 \w 1.00 54.00 0.50 17.00 -- 11.71 -99.00 -90.00 106
 14 \w 31.00 77.00 0.50 17.00 -- 11.71-139.00 -30.00 92
 15 \w -18.00 45.00 0.50 17.00 -- 11.71 -77.00-180.00 126
 16 \w 56.00 83.00 0.50 17.00 -- 11.71-179.00-180.00 54
 17 \w 1.00 54.00 0.50 17.00 -- 11.71 -99.00 60.00 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016361000
_diffrn_orient_matrix_UB_12      -0.0273944000
_diffrn_orient_matrix_UB_13      -0.0010371000
_diffrn_orient_matrix_UB_21      0.0328317000
_diffrn_orient_matrix_UB_22      -0.0000218000
_diffrn_orient_matrix_UB_23      0.0504849000
_diffrn_orient_matrix_UB_31      -0.0532134000
_diffrn_orient_matrix_UB_32      -0.0008638000
_diffrn_orient_matrix_UB_33      0.0311078000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9759
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26906
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9429
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1635.576
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.1118
_refine_diff_density_min         -0.1238
_refine_diff_density_rms         0.0241
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_d_res_high            0.7214
_refine_ls_d_res_low             5.9539
_refine_ls_goodness_of_fit_ref   1.0697
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0697
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0138
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.3599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0317
_reflns_Friedel_coverage         0.907
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              35
_reflns_limit_k_min              -34
_reflns_limit_l_max              16
_reflns_limit_l_min              -15
_reflns_number_gt                2263
_reflns_number_total             2327
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1sc06372c2.cif
_cod_data_source_block           pg156
_cod_depositor_comments
'Adding full bibliography for 1566274--1566277.cif.'
_cod_original_cell_volume        3509.66(13)
_cod_original_sg_symbol_Hall     ' F 2 -2d'
_cod_database_code               1566274
_chemical_oxdiff_formula         'Fe1 C24 H18 O2'
_chemical_oxdiff_usercomment     AK976-CDCl3-h
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2021-02-24
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.905