Chiral tetrahedral iron(II) cages: diastereoselective subcomponent self-assembly, structure interconversion and spin-crossover properties
Dong-Hong Ren; Dan Qiu; Chun-Yan Pang; Zaijun Li; Zhi-Guo Gu; Chem.Commun. 51 (2015) 788–; doi:10.1039/C4cc08041F

data_7116401
_publ_section_title
;
 Chiral tetrahedral iron(II) cages: diastereoselective subcomponent
 self-assembly, structure interconversion and spin-crossover properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              788
_journal_paper_doi               10.1039/C4cc08041F
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C180 H216 Fe4 N36 O12, 8(Cl O4), 2(C4 H10 O), 11.59(C2 H3 N), H2 O'
_chemical_formula_sum            'C211.17 H272.75 Cl8 Fe4 N47.58 O47'
_chemical_formula_weight         4736.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.6207(11)
_cell_angle_beta                 115.5608(12)
_cell_angle_gamma                94.4565(13)
_cell_formula_units_Z            1
_cell_length_a                   19.6065(9)
_cell_length_b                   19.7357(8)
_cell_length_c                   20.2252(9)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.99
_cell_volume                     5944.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51620
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.8936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2489
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.036(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2652
_refine_ls_number_reflns         33456
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1245P)^2^+4.8930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2337
_reflns_number_gt                22953
_reflns_number_total             33456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08041f2.cif
_cod_data_source_block           2R
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7116401