#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:53:29 +0100 (jue 07 de nov de 2019) $
#$Revision: 223884 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/12/7701208.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7701208
loop_
_publ_author_name
'Bodenstein, Tilmann'
'Eichhöfer, Andreas'
_publ_section_title
;
 Magnetic anisotropy in trigonal planar Fe(ii) bis(trimethylsilyl)amido
 complexes of the type
 [Fe{N(SiMe₃)₂}₂L]-experiment and theory.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15699
_journal_page_last               15712
_journal_paper_doi               10.1039/c9dt01702j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C17 H41 Fe N3 Si4'
_chemical_formula_weight         455.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-03-11 deposited with the CCDC.    2019-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   11.0457(3)
_cell_length_b                   34.2300(13)
_cell_length_c                   10.6870(3)
_cell_measurement_reflns_used    23669
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.19
_cell_volume                     4040.7(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15719
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_min         2.194
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.8008
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XRED32
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       Block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0791P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6171
_reflns_number_total             7119
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01702j2.cif
_cod_data_source_block           P21212
_cod_depositor_comments
'Adding full bibliography for 7701207--7701211.cif.'
_cod_database_code               7701208
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.01712(6) 0.17117(2) 0.80996(5) 0.04687(18) Uani 1 1 d . . .
Si1 Si 0.24853(14) 0.13978(4) 0.67662(13) 0.0560(3) Uani 1 1 d . . .
Si2 Si 0.03872(14) 0.08459(3) 0.71886(12) 0.0519(3) Uani 1 1 d . . .
Si3 Si -0.02719(14) 0.26229(3) 0.81063(12) 0.0533(3) Uani 1 1 d . . .
Si4 Si -0.20652(14) 0.20755(4) 0.68641(13) 0.0560(3) Uani 1 1 d . . .
N1 N 0.1070(4) 0.12940(10) 0.7333(3) 0.0501(9) Uani 1 1 d . . .
N2 N -0.0815(4) 0.21656(10) 0.7765(3) 0.0500(9) Uani 1 1 d . . .
N3 N 0.0199(4) 0.16346(10) 1.0050(3) 0.0512(9) Uani 1 1 d . . .
C1 C 0.2771(8) 0.19336(17) 0.6744(8) 0.106(3) Uani 1 1 d . . .
H1A H 0.2117 0.2065 0.6288 0.159 Uiso 1 1 calc R U .
H1B H 0.3544 0.1986 0.6327 0.159 Uiso 1 1 calc R U .
H1C H 0.2801 0.2032 0.7604 0.159 Uiso 1 1 calc R U .
C2 C 0.2732(7) 0.1220(2) 0.5152(6) 0.089(2) Uani 1 1 d . . .
H2A H 0.2673 0.0934 0.5139 0.134 Uiso 1 1 calc R U .
H2B H 0.3538 0.1299 0.4866 0.134 Uiso 1 1 calc R U .
H2C H 0.2116 0.1331 0.4598 0.134 Uiso 1 1 calc R U .
C3 C 0.3701(7) 0.1180(3) 0.7767(9) 0.105(2) Uani 1 1 d . . .
H3A H 0.3591 0.1266 0.8635 0.158 Uiso 1 1 calc R U .
H3B H 0.4494 0.1266 0.7464 0.158 Uiso 1 1 calc R U .
H3C H 0.3652 0.0895 0.7728 0.158 Uiso 1 1 calc R U .
C4 C -0.0496(7) 0.08036(17) 0.5704(5) 0.0780(18) Uani 1 1 d . . .
H4A H -0.1073 0.1020 0.5647 0.117 Uiso 1 1 calc R U .
H4B H -0.0937 0.0555 0.5697 0.117 Uiso 1 1 calc R U .
H4C H 0.0059 0.0813 0.4989 0.117 Uiso 1 1 calc R U .
C5 C 0.1487(6) 0.04316(13) 0.7215(6) 0.0684(15) Uani 1 1 d . . .
H5A H 0.2033 0.0452 0.6496 0.103 Uiso 1 1 calc R U .
H5B H 0.1045 0.0184 0.7173 0.103 Uiso 1 1 calc R U .
H5C H 0.1959 0.0441 0.7991 0.103 Uiso 1 1 calc R U .
C6 C -0.0674(6) 0.07531(16) 0.8519(6) 0.0721(16) Uani 1 1 d . . .
H6A H -0.0208 0.0707 0.9286 0.108 Uiso 1 1 calc R U .
H6B H -0.1170 0.0523 0.8334 0.108 Uiso 1 1 calc R U .
H6C H -0.1201 0.0981 0.8635 0.108 Uiso 1 1 calc R U .
C7 C 0.1157(6) 0.25974(15) 0.9038(6) 0.0750(16) Uani 1 1 d . . .
H7A H 0.1028 0.2433 0.9778 0.113 Uiso 1 1 calc R U .
H7B H 0.1390 0.2861 0.9303 0.113 Uiso 1 1 calc R U .
H7C H 0.1802 0.2485 0.8523 0.113 Uiso 1 1 calc R U .
C8 C -0.1331(7) 0.29183(16) 0.9083(6) 0.0787(18) Uani 1 1 d . . .
H8A H -0.2066 0.2975 0.8603 0.118 Uiso 1 1 calc R U .
H8B H -0.0938 0.3164 0.9321 0.118 Uiso 1 1 calc R U .
H8C H -0.1544 0.2771 0.9838 0.118 Uiso 1 1 calc R U .
C9 C 0.0064(8) 0.29060(17) 0.6649(6) 0.0809(17) Uani 1 1 d . . .
H9A H 0.0599 0.2752 0.6108 0.121 Uiso 1 1 calc R U .
H9B H 0.0463 0.3152 0.6871 0.121 Uiso 1 1 calc R U .
H9C H -0.0693 0.2962 0.6206 0.121 Uiso 1 1 calc R U .
C10 C -0.3182(6) 0.2485(2) 0.6836(7) 0.0873(19) Uani 1 1 d . . .
H10A H -0.3509 0.2525 0.7679 0.131 Uiso 1 1 calc R U .
H10B H -0.3844 0.2420 0.6262 0.131 Uiso 1 1 calc R U .
H10C H -0.2781 0.2724 0.6554 0.131 Uiso 1 1 calc R U .
C11 C -0.1613(6) 0.1978(2) 0.5206(5) 0.0776(17) Uani 1 1 d . . .
H11A H -0.1300 0.2218 0.4829 0.116 Uiso 1 1 calc R U .
H11B H -0.2319 0.1887 0.4732 0.116 Uiso 1 1 calc R U .
H11C H -0.0983 0.1776 0.5189 0.116 Uiso 1 1 calc R U .
C12 C -0.2887(7) 0.1633(2) 0.7409(8) 0.096(2) Uani 1 1 d . . .
H12A H -0.2334 0.1409 0.7407 0.143 Uiso 1 1 calc R U .
H12B H -0.3569 0.1580 0.6847 0.143 Uiso 1 1 calc R U .
H12C H -0.3190 0.1676 0.8259 0.143 Uiso 1 1 calc R U .
C13 C 0.0977(5) 0.13886(13) 1.0614(5) 0.0533(11) Uani 1 1 d . . .
H13 H 0.1521 0.1242 1.0112 0.064 Uiso 1 1 calc R U .
C14 C 0.1011(5) 0.13421(14) 1.1890(5) 0.0598(12) Uani 1 1 d . . .
H14 H 0.1578 0.1169 1.2263 0.072 Uiso 1 1 calc R U .
C15 C 0.0221(6) 0.15483(15) 1.2615(5) 0.0638(14) Uani 1 1 d . . .
H15 H 0.0231 0.1519 1.3499 0.077 Uiso 1 1 calc R U .
C16 C -0.0598(5) 0.18011(15) 1.2051(5) 0.0620(13) Uani 1 1 d . . .
H16 H -0.1160 0.1946 1.2538 0.074 Uiso 1 1 calc R U .
C17 C -0.0572(5) 0.18355(13) 1.0772(5) 0.0545(12) Uani 1 1 d . . .
H17 H -0.1126 0.2009 1.0381 0.065 Uiso 1 1 calc R U .
Fe2 Fe 0.5000 0.0000 0.11731(8) 0.0461(2) Uani 1 2 d S T P
Si5 Si 0.75932(13) 0.01517(3) 0.21233(11) 0.0472(3) Uani 1 1 d . . .
Si6 Si 0.58460(13) 0.08296(3) 0.21296(13) 0.0513(3) Uani 1 1 d . . .
N4 N 0.6212(4) 0.03570(10) 0.1762(4) 0.0471(8) Uani 1 1 d . . .
N5 N 0.5000 0.0000 -0.0806(5) 0.0604(14) Uani 1 2 d S T P
C18 C 0.8840(5) 0.05147(15) 0.2296(5) 0.0614(12) Uani 1 1 d . . .
H18A H 0.8976 0.0646 0.1494 0.092 Uiso 1 1 calc R U .
H18B H 0.9583 0.0380 0.2554 0.092 Uiso 1 1 calc R U .
H18C H 0.8617 0.0708 0.2931 0.092 Uiso 1 1 calc R U .
C19 C 0.8072(5) -0.01853(15) 0.0831(5) 0.0596(12) Uani 1 1 d . . .
H19A H 0.7403 -0.0362 0.0624 0.089 Uiso 1 1 calc R U .
H19B H 0.8774 -0.0338 0.1103 0.089 Uiso 1 1 calc R U .
H19C H 0.8289 -0.0032 0.0090 0.089 Uiso 1 1 calc R U .
C20 C 0.7532(6) -0.01166(15) 0.3643(5) 0.0656(14) Uani 1 1 d . . .
H20A H 0.7401 0.0070 0.4326 0.098 Uiso 1 1 calc R U .
H20B H 0.8298 -0.0255 0.3777 0.098 Uiso 1 1 calc R U .
H20C H 0.6866 -0.0305 0.3624 0.098 Uiso 1 1 calc R U .
C21 C 0.6727(6) 0.11877(15) 0.1190(7) 0.0796(18) Uani 1 1 d . . .
H21A H 0.7578 0.1180 0.1447 0.119 Uiso 1 1 calc R U .
H21B H 0.6402 0.1451 0.1326 0.119 Uiso 1 1 calc R U .
H21C H 0.6665 0.1121 0.0300 0.119 Uiso 1 1 calc R U .
C22 C 0.4223(5) 0.09362(14) 0.1762(6) 0.0678(14) Uani 1 1 d . . .
H22A H 0.4093 0.0915 0.0858 0.102 Uiso 1 1 calc R U .
H22B H 0.4023 0.1201 0.2039 0.102 Uiso 1 1 calc R U .
H22C H 0.3704 0.0748 0.2197 0.102 Uiso 1 1 calc R U .
C23 C 0.6054(7) 0.09323(16) 0.3835(6) 0.0745(16) Uani 1 1 d . . .
H23A H 0.5509 0.0766 0.4323 0.112 Uiso 1 1 calc R U .
H23B H 0.5869 0.1207 0.4003 0.112 Uiso 1 1 calc R U .
H23C H 0.6894 0.0878 0.4073 0.112 Uiso 1 1 calc R U .
C24 C 0.5734(6) 0.02400(18) -0.1451(6) 0.0733(16) Uani 1 1 d . . .
H24 H 0.6263 0.0410 -0.1008 0.088 Uiso 1 1 calc R U .
C25 C 0.5739(7) 0.0246(2) -0.2741(6) 0.089(2) Uani 1 1 d . . .
H25 H 0.6256 0.0421 -0.3179 0.107 Uiso 1 1 calc R U .
C26 C 0.5000 0.0000 -0.3381(8) 0.101(4) Uani 1 2 d S T P
H26 H 0.5000 0.0000 -0.4270 0.121 Uiso 1 2 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 N2 144.14(16) . .
N1 Fe1 N3 108.75(16) . .
N2 Fe1 N3 107.03(15) . .
N1 Si1 C2 113.3(3) . .
N1 Si1 C1 111.3(3) . .
C2 Si1 C1 106.7(3) . .
N1 Si1 C3 111.7(3) . .
C2 Si1 C3 107.2(4) . .
C1 Si1 C3 106.1(4) . .
N1 Si2 C5 113.1(3) . .
N1 Si2 C4 112.0(2) . .
C5 Si2 C4 107.1(3) . .
N1 Si2 C6 111.0(2) . .
C5 Si2 C6 105.5(3) . .
C4 Si2 C6 107.8(3) . .
N2 Si3 C8 113.2(3) . .
N2 Si3 C7 111.5(2) . .
C8 Si3 C7 104.9(3) . .
N2 Si3 C9 111.4(2) . .
C8 Si3 C9 108.0(3) . .
C7 Si3 C9 107.5(3) . .
N2 Si4 C12 111.4(3) . .
N2 Si4 C10 114.0(3) . .
C12 Si4 C10 107.1(4) . .
N2 Si4 C11 110.5(3) . .
C12 Si4 C11 106.3(4) . .
C10 Si4 C11 107.2(3) . .
Si1 N1 Si2 123.7(2) . .
Si1 N1 Fe1 117.8(2) . .
Si2 N1 Fe1 118.4(2) . .
Si4 N2 Si3 124.5(2) . .
Si4 N2 Fe1 114.46(19) . .
Si3 N2 Fe1 119.8(2) . .
C17 N3 C13 118.0(4) . .
C17 N3 Fe1 119.9(3) . .
C13 N3 Fe1 122.2(3) . .
N3 C13 C14 122.4(5) . .
C15 C14 C13 119.1(5) . .
C14 C15 C16 119.5(5) . .
C17 C16 C15 118.2(5) . .
N3 C17 C16 122.9(5) . .
N4 Fe2 N4 141.7(2) . 2_655
N4 Fe2 N5 109.14(11) . .
N4 Fe2 N5 109.14(11) 2_655 .
N4 Si5 C18 113.9(2) . .
N4 Si5 C20 111.3(2) . .
C18 Si5 C20 105.6(3) . .
N4 Si5 C19 109.6(2) . .
C18 Si5 C19 105.9(2) . .
C20 Si5 C19 110.4(2) . .
N4 Si6 C21 112.0(2) . .
N4 Si6 C23 111.8(2) . .
C21 Si6 C23 109.8(3) . .
N4 Si6 C22 111.2(2) . .
C21 Si6 C22 105.0(3) . .
C23 Si6 C22 106.6(3) . .
Si6 N4 Si5 122.8(2) . .
Si6 N4 Fe2 120.8(2) . .
Si5 N4 Fe2 115.57(18) . .
C24 N5 C24 118.3(7) 2_655 .
C24 N5 Fe2 120.9(4) 2_655 .
C24 N5 Fe2 120.8(4) . .
N5 C24 C25 121.6(7) . .
C26 C25 C24 119.5(8) . .
C25 C26 C25 119.5(8) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.924(4) .
Fe1 N2 1.931(4) .
Fe1 N3 2.101(4) .
Si1 N1 1.714(4) .
Si1 C2 1.850(6) .
Si1 C1 1.861(6) .
Si1 C3 1.871(8) .
Si2 N1 1.716(4) .
Si2 C5 1.867(5) .
Si2 C4 1.868(6) .
Si2 C6 1.870(6) .
Si3 N2 1.715(4) .
Si3 C8 1.866(6) .
Si3 C7 1.868(6) .
Si3 C9 1.871(6) .
Si4 N2 1.712(4) .
Si4 C12 1.861(7) .
Si4 C10 1.867(6) .
Si4 C11 1.871(6) .
N3 C17 1.340(6) .
N3 C13 1.345(6) .
C13 C14 1.374(7) .
C14 C15 1.364(8) .
C15 C16 1.389(8) .
C16 C17 1.373(7) .
Fe2 N4 1.918(4) .
Fe2 N4 1.918(4) 2_655
Fe2 N5 2.115(6) .
Si5 N4 1.724(4) .
Si5 C18 1.864(5) .
Si5 C20 1.867(5) .
Si5 C19 1.876(5) .
Si6 N4 1.713(3) .
Si6 C21 1.860(6) .
Si6 C23 1.870(6) .
Si6 C22 1.871(6) .
N5 C24 1.345(7) 2_655
N5 C24 1.345(7) .
C24 C25 1.378(9) .
C25 C26 1.357(9) .
C26 C25 1.358(9) 2_655
