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_1566275
_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_formula_sum            'C69 H75 Cl9 Fe3 N6 O0.39'
_chemical_formula_weight         1481.20
_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     shelxt
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                97.399(2)
_cell_angle_beta                 93.732(2)
_cell_angle_gamma                113.532(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1378(3)
_cell_length_b                   16.3059(3)
_cell_length_c                   19.0267(3)
_cell_measurement_reflns_used    20985
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7580
_cell_measurement_theta_min      2.9840
_cell_volume                     3675.33(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59203
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.452
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1530
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00056(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         14936
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0947P)^2^+2.2232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10962
_reflns_number_total             14936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06372c2.cif
_cod_data_source_block           pms2_auto_sq
_cod_depositor_comments
'Adding full bibliography for 1566274--1566277.cif.'
_cod_original_cell_volume        3675.33(13)
_cod_database_code               1566275
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              7364
_shelx_fab_checksum              46130