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_7116400
_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         'C168 H192 Fe4 N36, 8(Cl O4)'
_chemical_formula_sum            'C168 H192 Cl8 Fe4 N36 O32'
_chemical_formula_weight         3734.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   30.825(8)
_cell_length_b                   30.825(8)
_cell_length_c                   22.939(11)
_cell_measurement_reflns_used    2425
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      3.18
_cell_volume                     18876(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.776
_diffrn_measured_fraction_theta_max 0.776
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.1354
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7838
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5844
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_platon_squeeze_details
;
;
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         7330
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.1395
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3552
_refine_ls_wR_factor_ref         0.3745
_reflns_number_gt                4998
_reflns_number_total             7330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08041f2.cif
_cod_data_source_block           1S
_cod_original_cell_volume        18877(12)
_cod_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7116400