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_1566276
_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            'C113 H114 Cl18 Fe3 N6'
_chemical_formula_weight         2361.76
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_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
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_cell_length_b                   17.0394(2)
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_cell_measurement_reflns_used    40746
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      1.9830
_cell_volume                     5519.49(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            106018
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         30.837
_diffrn_reflns_theta_min         1.979
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2436
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_refine_ls_number_reflns         28532
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_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+8.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22150
_reflns_number_total             28532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06372c2.cif
_cod_data_source_block           PMS5_auto
_cod_depositor_comments
'Adding full bibliography for 1566274--1566277.cif.'
_cod_original_cell_volume        5519.48(17)
_cod_database_code               1566276
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.64792
_shelx_estimated_absorpt_t_max   1.00000
_shelx_res_checksum              14364