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_7120340
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                82.518(2)
_cell_angle_beta                 80.847(2)
_cell_angle_gamma                62.5150(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7108(4)
_cell_length_b                   12.8539(4)
_cell_length_c                   21.7124(7)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.45
_cell_volume                     3100.44(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.756
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.756
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            110784
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.171
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       rod
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         19392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0502P)^2^+2.7906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15411
_reflns_number_total             19392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04670g2.cif
_cod_data_source_block           all
_cod_database_code               7120340
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              63041