A High-Spin Square Planar Iron(II)-Siloxide and its Tetrahedral Allogon – Structural and Spectroscopic Models of Fe-Zeolite Sites
Limberg, Christian; Pinkert, Denise; Keck, Matthias; Ghassemi Tabrizi, Shadan; Beckmann, Fabian; Braun, Beatrice; Herwig, Christian; Kaupp, Martin; Chem. Commun.  (2017) –; doi:10.1039/C7CC04670G

data_7120339
_publ_section_title
;
 A High-Spin Square Planar Iron(II)-Siloxide and its Tetrahedral Allogon
 -- Structural and Spectroscopic Models of Fe-Zeolite Sites
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04670G
_journal_year                    2017
_chemical_formula_moiety         'C64 H72 Fe Li2 O10 Si4'
_chemical_formula_sum            'C64 H72 Fe Li2 O10 Si4'
_chemical_formula_weight         1183.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0163(7)
_cell_length_b                   14.0910(3)
_cell_length_c                   20.0026(6)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.32
_cell_volume                     6238.8(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39208
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.197
_diffrn_reflns_theta_min         3.316
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Spek, 2003'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_exptl_transmission_factor_max   0.914
_exptl_transmission_factor_min   0.882
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 4812 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.390(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         15812
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.908
_reflns_Friedel_fraction_max     0.876
_reflns_number_gt                12570
_reflns_number_total             15812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04670g2.cif
_cod_data_source_block           dn320blue
_cod_database_code               7120339
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.916
_shelxl_version_number           2013-4
_shelx_res_checksum              85458