A three-coordinate iron-silylene complex stabilized by ligand-ligand dispersion forces.
Hänninen, Mikko M; Pal, Kuntal; Day, Benjamin M.; Pugh, Thomas; Layfield, Richard A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11301–11305; doi:10.1039/c6dt02486f

data_7039696
_publ_section_title
;
 A three-coordinate iron-silylene complex stabilized by ligand-ligand
 dispersion forces.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11301
_journal_page_last               11305
_journal_paper_doi               10.1039/c6dt02486f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C38 H72 Fe N4 Si5), C7 H8'
_chemical_formula_sum            'C83 H152 Fe2 N8 Si10'
_chemical_formula_weight         1654.72
_chemical_name_systematic        (NHSi)Fe(N{SiMe3}2)2
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                78.705(3)
_cell_angle_beta                 89.821(3)
_cell_angle_gamma                75.266(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3552(4)
_cell_length_b                   12.5187(4)
_cell_length_c                   18.5545(6)
_cell_measurement_reflns_used    10489
_cell_measurement_temperature    150.01(13)
_cell_measurement_theta_max      27.2360
_cell_measurement_theta_min      3.6520
_cell_volume                     2498.40(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -88.00   12.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000 -150.0000 100

  2 omega  -91.00   26.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -19.0000   30.0000 117

  3 omega  -48.00   52.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   77.0000  -30.0000 100

  4 omega  -94.00  -35.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -60.0000 59

  5 omega  -20.00   61.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -99.0000  120.0000 81

  6 omega  -94.00  -34.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  178.0000  120.0000 60

  7 omega  -87.00  -62.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000 -120.0000 25

  8 omega  -90.00    8.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -37.0000  -60.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      -0.0546682000
_diffrn_orient_matrix_UB_12      -0.0034816000
_diffrn_orient_matrix_UB_13      -0.0166652000
_diffrn_orient_matrix_UB_21      0.0193579000
_diffrn_orient_matrix_UB_22      0.0210528000
_diffrn_orient_matrix_UB_23      -0.0350930000
_diffrn_orient_matrix_UB_31      0.0286088000
_diffrn_orient_matrix_UB_32      -0.0558792000
_diffrn_orient_matrix_UB_33      -0.0037564000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31256
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10197
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0358P)^2^+1.6763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7910
_reflns_number_total             10197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02486f2.cif
_cod_data_source_block           NHSiFe
_cod_depositor_comments          'Adding full bibliography for 7039696.cif.'
_cod_database_code               7039696
_chemical_oxdiff_formula         C83H152N8Si10Fe2
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C39, C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C40(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5)
 C44(0.5) H44(0.5) C39(0.5) H39(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19),
 C41(H41), C42(H42), C43(H43), C44(H44), C39(H39)
5.c Fitted hexagon refined as free rotating group:
 C40(C41,C42,C43,C44,C39)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              30606
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene