#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:57:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178762 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/16/4101649.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_4101649
loop_
_publ_author_name
'Miller, Kevin L.'
'Williams, Bryan N.'
'Benitez, Diego'
'Carver, Colin T.'
'Ogilby, Kevin R.'
'Tkatchouk, Ekaterina'
'Goddard, 3rd, William A.'
'Diaconescu, Paula L.'
_publ_section_title
;
 Dearomatization reactions of N-heterocycles mediated by group 3
 complexes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              342
_journal_page_last               355
_journal_paper_doi               10.1021/ja908489p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C49 H60 Fe Lu N5 Si2, 0.5(C6 H8)'
_chemical_formula_sum            'C52 H64 Fe Lu N5 Si2'
_chemical_formula_weight         1046.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.659(2)
_cell_angle_beta                 116.825(2)
_cell_angle_gamma                98.466(2)
_cell_formula_units_Z            2
_cell_length_a                   13.908(2)
_cell_length_b                   13.942(5)
_cell_length_c                   14.914(3)
_cell_measurement_reflns_used    7681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      3.99
_cell_volume                     2507.6(11)
_computing_cell_refinement       'Bruker APEX11'
_computing_data_collection       'Bruker APEX11'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22108
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.9125
_exptl_absorpt_correction_T_min  0.7672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         12008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0330P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                10156
_reflns_number_total             12008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja908489p_si_002.cif
_cod_data_source_block           4Lu-(iqn)2
_cod_original_cell_volume        2507.6(10)
_cod_database_code               4101649
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.894903(10) 0.775489(9) 0.696800(9) 0.01933(4) Uani 1 1 d . . .
Fe1 Fe 0.84006(3) 0.54433(3) 0.56396(3) 0.02087(9) Uani 1 1 d . . .
Si1 Si 0.61198(6) 0.77481(6) 0.50013(6) 0.02205(17) Uani 1 1 d . . .
Si2 Si 1.08835(8) 0.68565(7) 0.91235(7) 0.0303(2) Uani 1 1 d . . .
C1 C 0.8949(3) 0.9969(2) 0.7879(2) 0.0302(7) Uani 1 1 d . . .
H1A H 0.8266 0.9686 0.7846 0.036 Uiso 1 1 calc R . .
N3 N 1.0148(2) 0.82107(18) 0.62189(19) 0.0262(6) Uani 1 1 d . . .
N4 N 0.7968(2) 0.75432(18) 0.79595(18) 0.0244(5) Uani 1 1 d . . .
N2 N 1.0067(2) 0.68313(17) 0.78386(18) 0.0231(5) Uani 1 1 d . . .
N1 N 0.73623(18) 0.73787(17) 0.55148(17) 0.0198(5) Uani 1 1 d . . .
N5 N 0.9561(2) 0.93358(18) 0.77688(18) 0.0244(5) Uani 1 1 d . . .
C19 C 0.7384(2) 0.6455(2) 0.5045(2) 0.0199(6) Uani 1 1 d . . .
C23 C 0.6765(2) 0.5494(2) 0.4971(2) 0.0232(6) Uani 1 1 d . . .
H23A H 0.6264 0.5358 0.5279 0.028 Uiso 1 1 calc R . .
C14 C 0.9783(3) 0.8631(2) 0.5360(2) 0.0278(7) Uani 1 1 d . . .
H14A H 0.9083 0.8803 0.5109 0.033 Uiso 1 1 calc R . .
C17 C 1.1837(2) 0.8186(2) 0.6126(2) 0.0265(7) Uani 1 1 d . . .
C21 C 0.7731(2) 0.5267(2) 0.4087(2) 0.0253(6) Uani 1 1 d . . .
H21A H 0.8027 0.4950 0.3662 0.030 Uiso 1 1 calc R . .
C20 C 0.8003(2) 0.6286(2) 0.4513(2) 0.0211(6) Uani 1 1 d . . .
H20A H 0.8536 0.6804 0.4450 0.025 Uiso 1 1 calc R . .
C22 C 0.6971(2) 0.4776(2) 0.4368(2) 0.0258(7) Uani 1 1 d . . .
H22A H 0.6631 0.4053 0.4170 0.031 Uiso 1 1 calc R . .
C6 C 1.0723(2) 0.9847(2) 0.8203(2) 0.0246(6) Uani 1 1 d . . .
H6A H 1.1119 0.9417 0.7992 0.030 Uiso 1 1 calc R . .
H6B H 1.1065 0.9959 0.8959 0.030 Uiso 1 1 calc R . .
C7 C 0.7110(2) 0.6792(2) 0.7617(2) 0.0238(6) Uani 1 1 d . . .
H7A H 0.6853 0.6417 0.6954 0.029 Uiso 1 1 calc R . .
C5 C 1.1714(3) 1.1180(2) 0.7662(2) 0.0289(7) Uani 1 1 d . . .
H5A H 1.2191 1.0766 0.7638 0.035 Uiso 1 1 calc R . .
C30 C 0.5663(2) 0.8026(2) 0.3657(2) 0.0258(6) Uani 1 1 d . . .
C8 C 0.6552(2) 0.6513(2) 0.8176(2) 0.0223(6) Uani 1 1 d . . .
C15 C 1.0374(3) 0.8814(2) 0.4850(2) 0.0301(7) Uani 1 1 d . . .
H15A H 1.0085 0.9100 0.4255 0.036 Uiso 1 1 calc R . .
C16 C 1.1423(2) 0.8573(2) 0.5219(2) 0.0267(7) Uani 1 1 d . . .
C2 C 0.9226(3) 1.0971(2) 0.8033(2) 0.0303(7) Uani 1 1 d . . .
H2A H 0.8828 1.1367 0.8230 0.036 Uiso 1 1 calc R . .
C29 C 0.6272(3) 0.8890(2) 0.5863(2) 0.0306(7) Uani 1 1 d . . .
H29A H 0.6401 0.8736 0.6530 0.046 Uiso 1 1 calc R . .
H29B H 0.5597 0.9146 0.5560 0.046 Uiso 1 1 calc R . .
H29C H 0.6899 0.9389 0.5952 0.046 Uiso 1 1 calc R . .
C10 C 0.7870(3) 0.7857(2) 0.9523(2) 0.0282(7) Uani 1 1 d . . .
H10A H 0.8164 0.8241 1.0188 0.034 Uiso 1 1 calc R . .
C28 C 0.8857(3) 0.5090(2) 0.7064(2) 0.0266(7) Uani 1 1 d . . .
H28A H 0.8406 0.5084 0.7430 0.032 Uiso 1 1 calc R . .
C4 C 1.0865(2) 1.0826(2) 0.7874(2) 0.0244(6) Uani 1 1 d . . .
C26 C 0.9548(3) 0.4596(2) 0.5999(2) 0.0305(7) Uani 1 1 d . . .
H26A H 0.9688 0.4181 0.5502 0.037 Uiso 1 1 calc R . .
C25 C 1.0075(2) 0.5595(2) 0.6470(2) 0.0252(6) Uani 1 1 d . . .
H25A H 1.0640 0.6008 0.6348 0.030 Uiso 1 1 calc R . .
C3 C 1.0140(3) 1.1422(2) 0.7887(2) 0.0269(7) Uani 1 1 d . . .
C9 C 0.6952(2) 0.7072(2) 0.9170(2) 0.0245(6) Uani 1 1 d . . .
C27 C 0.8795(3) 0.4286(2) 0.6368(2) 0.0318(7) Uani 1 1 d . . .
H27A H 0.8309 0.3615 0.6173 0.038 Uiso 1 1 calc R . .
C13 C 0.5506(3) 0.6042(2) 0.9334(2) 0.0316(7) Uani 1 1 d . . .
H13A H 0.5144 0.5874 0.9724 0.038 Uiso 1 1 calc R . .
C12 C 0.6405(3) 0.6806(2) 0.9744(2) 0.0311(7) Uani 1 1 d . . .
H12A H 0.6666 0.7162 1.0416 0.037 Uiso 1 1 calc R . .
C35 C 1.1492(3) 0.8175(2) 0.9782(2) 0.0336(8) Uani 1 1 d . . .
H35A H 1.0897 0.8529 0.9657 0.050 Uiso 1 1 calc R . .
H35B H 1.1964 0.8482 0.9515 0.050 Uiso 1 1 calc R . .
H35C H 1.1932 0.8206 1.0519 0.050 Uiso 1 1 calc R . .
C24 C 0.9679(2) 0.5913(2) 0.7167(2) 0.0249(6) Uani 1 1 d . . .
C11 C 0.8341(3) 0.8073(2) 0.8921(2) 0.0282(7) Uani 1 1 d . . .
H11A H 0.8955 0.8614 0.9178 0.034 Uiso 1 1 calc R . .
C34 C 1.0086(3) 0.6282(3) 0.9736(3) 0.0458(10) Uani 1 1 d . . .
H34A H 0.9544 0.6669 0.9712 0.069 Uiso 1 1 calc R . .
H34B H 1.0594 0.6270 1.0450 0.069 Uiso 1 1 calc R . .
H34C H 0.9703 0.5606 0.9367 0.069 Uiso 1 1 calc R . .
C18 C 1.1139(2) 0.8019(2) 0.6588(2) 0.0268(7) Uani 1 1 d . . .
H18A H 1.1407 0.7755 0.7198 0.032 Uiso 1 1 calc R . .
C32 C 0.6555(3) 0.8828(2) 0.3669(3) 0.0361(8) Uani 1 1 d . . .
H32A H 0.6331 0.8950 0.2974 0.054 Uiso 1 1 calc R . .
H32B H 0.7254 0.8609 0.3927 0.054 Uiso 1 1 calc R . .
H32C H 0.6649 0.9439 0.4115 0.054 Uiso 1 1 calc R . .
C33 C 0.4576(3) 0.8393(3) 0.3257(3) 0.0399(8) Uani 1 1 d . . .
H33A H 0.4367 0.8536 0.2571 0.060 Uiso 1 1 calc R . .
H33B H 0.4677 0.8995 0.3719 0.060 Uiso 1 1 calc R . .
H33C H 0.3992 0.7882 0.3228 0.060 Uiso 1 1 calc R . .
C31 C 0.5474(3) 0.7093(2) 0.2905(2) 0.0309(7) Uani 1 1 d . . .
H31A H 0.5307 0.7262 0.2235 0.046 Uiso 1 1 calc R . .
H31B H 0.4854 0.6601 0.2838 0.046 Uiso 1 1 calc R . .
H31C H 0.6141 0.6823 0.3162 0.046 Uiso 1 1 calc R . .
C49 C 0.5621(2) 0.5724(2) 0.7773(2) 0.0290(7) Uani 1 1 d . . .
H49A H 0.5354 0.5352 0.7107 0.035 Uiso 1 1 calc R . .
C36 C 0.4946(2) 0.6793(2) 0.4896(3) 0.0288(7) Uani 1 1 d . . .
H36A H 0.5134 0.6619 0.5568 0.043 Uiso 1 1 calc R . .
H36B H 0.4816 0.6202 0.4408 0.043 Uiso 1 1 calc R . .
H36C H 0.4277 0.7061 0.4658 0.043 Uiso 1 1 calc R . .
C46 C 1.1168(3) 1.2738(2) 0.7512(2) 0.0350(8) Uani 1 1 d . . .
H46A H 1.1278 1.3395 0.7399 0.042 Uiso 1 1 calc R . .
C45 C 1.1868(3) 1.2143(2) 0.7482(2) 0.0331(8) Uani 1 1 d . . .
H45A H 1.2450 1.2386 0.7340 0.040 Uiso 1 1 calc R . .
C44 C 1.2082(3) 0.8711(2) 0.4706(3) 0.0330(7) Uani 1 1 d . . .
H44A H 1.1812 0.8955 0.4084 0.040 Uiso 1 1 calc R . .
C47 C 1.0311(3) 1.2390(2) 0.7703(2) 0.0335(8) Uani 1 1 d . . .
H47A H 0.9831 1.2807 0.7712 0.040 Uiso 1 1 calc R . .
C48 C 0.5105(3) 0.5497(2) 0.8342(3) 0.0329(7) Uani 1 1 d . . .
H48A H 0.4474 0.4970 0.8068 0.040 Uiso 1 1 calc R . .
C43 C 1.3093(3) 0.8488(2) 0.5121(3) 0.0346(8) Uani 1 1 d . . .
H43A H 1.3533 0.8584 0.4788 0.042 Uiso 1 1 calc R . .
C42 C 1.3506(3) 0.8115(2) 0.6043(3) 0.0363(8) Uani 1 1 d . . .
H42A H 1.4220 0.7970 0.6322 0.044 Uiso 1 1 calc R . .
C41 C 1.2888(3) 0.7961(2) 0.6536(3) 0.0350(8) Uani 1 1 d . . .
H41A H 1.3167 0.7704 0.7150 0.042 Uiso 1 1 calc R . .
C37 C 1.2081(3) 0.6215(3) 0.9375(3) 0.0474(10) Uani 1 1 d . . .
C38 C 1.1668(4) 0.5086(3) 0.9032(3) 0.0541(11) Uani 1 1 d . . .
H38A H 1.2293 0.4779 0.9144 0.081 Uiso 1 1 calc R . .
H38B H 1.1127 0.4930 0.8304 0.081 Uiso 1 1 calc R . .
H38C H 1.1321 0.4833 0.9430 0.081 Uiso 1 1 calc R . .
C40 C 1.2703(3) 0.6598(3) 0.8808(3) 0.0600(12) Uani 1 1 d . . .
H40A H 1.3361 0.6320 0.9004 0.090 Uiso 1 1 calc R . .
H40B H 1.2923 0.7320 0.8990 0.090 Uiso 1 1 calc R . .
H40C H 1.2220 0.6400 0.8069 0.090 Uiso 1 1 calc R . .
C39 C 1.2886(4) 0.6421(4) 1.0528(3) 0.0783(17) Uani 1 1 d . . .
H39A H 1.3495 0.6086 1.0655 0.117 Uiso 1 1 calc R . .
H39B H 1.2497 0.6173 1.0895 0.117 Uiso 1 1 calc R . .
H39C H 1.3178 0.7133 1.0769 0.117 Uiso 1 1 calc R . .
C1S C 0.4016(5) 0.0485(4) 0.1511(4) 0.0726(14) Uani 1 1 d . . .
C3S C 0.4749(8) 0.0117(7) 0.0279(7) 0.153(4) Uani 1 1 d . . .
H3SA H 0.4921 0.0846 0.0380 0.183 Uiso 1 1 calc R A 1
H3SB H 0.3964 -0.0081 -0.0249 0.183 Uiso 1 1 calc R A 1
C2SA C 0.4670(8) -0.0009(6) 0.1096(7) 0.074(2) Uani 0.60 1 d P B 1
H2SA H 0.5438 0.0146 0.1660 0.089 Uiso 0.60 1 calc PR B 1
H2SB H 0.4397 -0.0727 0.1004 0.089 Uiso 0.60 1 calc PR B 1
C2SB C 0.4312(13) 0.0644(14) 0.0664(14) 0.100(5) Uani 0.40 1 d P B 2
H2SC H 0.3615 0.0700 0.0077 0.120 Uiso 0.40 1 calc PR B 2
H2SD H 0.4798 0.1310 0.0899 0.120 Uiso 0.40 1 calc PR B 2
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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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
_geom_angle_publ_flag
N2 Lu1 N1 131.64(9) . . ?
N2 Lu1 N5 111.07(9) . . ?
N1 Lu1 N5 117.26(9) . . ?
N2 Lu1 N4 90.24(9) . . ?
N1 Lu1 N4 90.95(8) . . ?
N5 Lu1 N4 86.67(9) . . ?
N2 Lu1 N3 89.18(9) . . ?
N1 Lu1 N3 96.99(8) . . ?
N5 Lu1 N3 84.10(9) . . ?
N4 Lu1 N3 169.87(8) . . ?
N2 Lu1 C24 28.24(8) . . ?
N1 Lu1 C24 103.82(8) . . ?
N5 Lu1 C24 138.78(9) . . ?
N4 Lu1 C24 96.29(8) . . ?
N3 Lu1 C24 87.95(9) . . ?
N2 Lu1 C19 104.64(8) . . ?
N1 Lu1 C19 28.30(8) . . ?
N5 Lu1 C19 143.48(8) . . ?
N4 Lu1 C19 100.83(8) . . ?
N3 Lu1 C19 89.10(8) . . ?
C24 Lu1 C19 76.41(8) . . ?
N2 Lu1 Fe1 66.53(6) . . ?
N1 Lu1 Fe1 66.22(6) . . ?
N5 Lu1 Fe1 169.49(6) . . ?
N4 Lu1 Fe1 103.40(6) . . ?
N3 Lu1 Fe1 85.63(6) . . ?
C24 Lu1 Fe1 38.31(6) . . ?
C19 Lu1 Fe1 38.24(5) . . ?
C22 Fe1 C26 111.92(12) . . ?
C22 Fe1 C27 101.21(13) . . ?
C26 Fe1 C27 40.87(13) . . ?
C22 Fe1 C21 40.73(12) . . ?
C26 Fe1 C21 102.59(12) . . ?
C27 Fe1 C21 121.05(13) . . ?
C22 Fe1 C23 40.95(11) . . ?
C26 Fe1 C23 147.53(12) . . ?
C27 Fe1 C23 115.50(13) . . ?
C21 Fe1 C23 68.46(12) . . ?
C22 Fe1 C25 148.21(12) . . ?
C26 Fe1 C25 40.65(12) . . ?
C27 Fe1 C25 68.32(13) . . ?
C21 Fe1 C25 117.66(12) . . ?
C23 Fe1 C25 170.68(12) . . ?
C22 Fe1 C28 124.01(13) . . ?
C26 Fe1 C28 68.28(13) . . ?
C27 Fe1 C28 40.40(12) . . ?
C21 Fe1 C28 159.64(12) . . ?
C23 Fe1 C28 108.93(12) . . ?
C25 Fe1 C28 67.98(12) . . ?
C22 Fe1 C20 68.31(12) . . ?
C26 Fe1 C20 125.87(12) . . ?
C27 Fe1 C20 160.34(12) . . ?
C21 Fe1 C20 40.42(11) . . ?
C23 Fe1 C20 68.14(11) . . ?
C25 Fe1 C20 111.37(12) . . ?
C28 Fe1 C20 159.08(12) . . ?
C22 Fe1 C19 68.48(11) . . ?
C26 Fe1 C19 165.80(12) . . ?
C27 Fe1 C19 153.04(13) . . ?
C21 Fe1 C19 68.02(11) . . ?
C23 Fe1 C19 40.63(10) . . ?
C25 Fe1 C19 133.10(12) . . ?
C28 Fe1 C19 124.05(12) . . ?
C20 Fe1 C19 40.22(11) . . ?
C22 Fe1 C24 163.98(12) . . ?
C26 Fe1 C24 68.21(12) . . ?
C27 Fe1 C24 67.97(12) . . ?
C21 Fe1 C24 154.99(12) . . ?
C23 Fe1 C24 131.67(12) . . ?
C25 Fe1 C24 40.44(11) . . ?
C28 Fe1 C24 40.24(11) . . ?
C20 Fe1 C24 125.48(12) . . ?
C19 Fe1 C24 115.60(11) . . ?
C22 Fe1 Lu1 125.57(8) . . ?
C26 Fe1 Lu1 122.40(9) . . ?
C27 Fe1 Lu1 121.34(9) . . ?
C21 Fe1 Lu1 117.54(9) . . ?
C23 Fe1 Lu1 87.79(8) . . ?
C25 Fe1 Lu1 83.08(8) . . ?
C28 Fe1 Lu1 81.94(9) . . ?
C20 Fe1 Lu1 77.29(8) . . ?
C19 Fe1 Lu1 58.11(8) . . ?
C24 Fe1 Lu1 57.77(8) . . ?
N1 Si1 C29 107.87(13) . . ?
N1 Si1 C36 112.81(13) . . ?
C29 Si1 C36 108.04(15) . . ?
N1 Si1 C30 113.72(13) . . ?
C29 Si1 C30 108.48(14) . . ?
C36 Si1 C30 105.73(14) . . ?
N2 Si2 C35 108.24(13) . . ?
N2 Si2 C34 112.61(16) . . ?
C35 Si2 C34 107.62(16) . . ?
N2 Si2 C37 112.39(14) . . ?
C35 Si2 C37 107.42(17) . . ?
C34 Si2 C37 108.32(18) . . ?
N5 C1 C2 125.9(3) . . ?
N5 C1 H1A 117.1 . . ?
C2 C1 H1A 117.1 . . ?
C18 N3 C14 117.8(3) . . ?
C18 N3 Lu1 121.3(2) . . ?
C14 N3 Lu1 120.7(2) . . ?
C7 N4 C11 117.4(3) . . ?
C7 N4 Lu1 118.51(19) . . ?
C11 N4 Lu1 123.43(19) . . ?
C24 N2 Si2 117.81(19) . . ?
C24 N2 Lu1 104.07(17) . . ?
Si2 N2 Lu1 134.11(13) . . ?
C19 N1 Si1 116.90(18) . . ?
C19 N1 Lu1 103.43(16) . . ?
Si1 N1 Lu1 137.90(13) . . ?
C1 N5 C6 110.5(2) . . ?
C1 N5 Lu1 127.1(2) . . ?
C6 N5 Lu1 122.28(18) . . ?
N1 C19 C20 126.7(2) . . ?
N1 C19 C23 127.4(2) . . ?
C20 C19 C23 105.9(2) . . ?
N1 C19 Fe1 130.94(19) . . ?
C20 C19 Fe1 67.87(15) . . ?
C23 C19 Fe1 67.11(16) . . ?
N1 C19 Lu1 48.27(13) . . ?
C20 C19 Lu1 105.43(17) . . ?
C23 C19 Lu1 123.86(19) . . ?
Fe1 C19 Lu1 83.65(9) . . ?
C22 C23 C19 108.6(3) . . ?
C22 C23 Fe1 68.89(16) . . ?
C19 C23 Fe1 72.26(16) . . ?
C22 C23 H23A 125.7 . . ?
C19 C23 H23A 125.7 . . ?
Fe1 C23 H23A 125.7 . . ?
C15 C14 N3 123.4(3) . . ?
C15 C14 H14A 118.3 . . ?
N3 C14 H14A 118.3 . . ?
C41 C17 C16 120.5(3) . . ?
C41 C17 C18 122.2(3) . . ?
C16 C17 C18 117.3(3) . . ?
C22 C21 C20 108.3(3) . . ?
C22 C21 Fe1 69.22(17) . . ?
C20 C21 Fe1 70.60(17) . . ?
C22 C21 H21A 125.8 . . ?
C20 C21 H21A 125.8 . . ?
Fe1 C21 H21A 125.8 . . ?
C21 C20 C19 109.1(3) . . ?
C21 C20 Fe1 68.98(17) . . ?
C19 C20 Fe1 71.91(16) . . ?
C21 C20 H20A 125.4 . . ?
C19 C20 H20A 125.4 . . ?
Fe1 C20 H20A 125.4 . . ?
C21 C22 C23 108.0(3) . . ?
C21 C22 Fe1 70.05(16) . . ?
C23 C22 Fe1 70.16(17) . . ?
C21 C22 H22A 126.0 . . ?
C23 C22 H22A 126.0 . . ?
Fe1 C22 H22A 126.0 . . ?
N5 C6 C4 113.2(2) . . ?
N5 C6 H6A 108.9 . . ?
C4 C6 H6A 108.9 . . ?
N5 C6 H6B 108.9 . . ?
C4 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
N4 C7 C8 124.2(3) . . ?
N4 C7 H7A 117.9 . . ?
C8 C7 H7A 117.9 . . ?
C4 C5 C45 120.2(3) . . ?
C4 C5 H5A 119.9 . . ?
C45 C5 H5A 119.9 . . ?
C32 C30 C31 108.9(3) . . ?
C32 C30 C33 108.4(3) . . ?
C31 C30 C33 107.8(3) . . ?
C32 C30 Si1 109.7(2) . . ?
C31 C30 Si1 110.5(2) . . ?
C33 C30 Si1 111.3(2) . . ?
C49 C8 C7 122.5(3) . . ?
C49 C8 C9 120.1(3) . . ?
C7 C8 C9 117.4(3) . . ?
C14 C15 C16 119.1(3) . . ?
C14 C15 H15A 120.4 . . ?
C16 C15 H15A 120.4 . . ?
C17 C16 C15 118.5(3) . . ?
C17 C16 C44 118.9(3) . . ?
C15 C16 C44 122.5(3) . . ?
C1 C2 C3 118.6(3) . . ?
C1 C2 H2A 120.7 . . ?
C3 C2 H2A 120.7 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C27 C28 C24 109.1(3) . . ?
C27 C28 Fe1 68.99(17) . . ?
C24 C28 Fe1 72.11(16) . . ?
C27 C28 H28A 125.4 . . ?
C24 C28 H28A 125.4 . . ?
Fe1 C28 H28A 125.4 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 C6 123.7(3) . . ?
C3 C4 C6 115.7(3) . . ?
C25 C26 C27 107.8(3) . . ?
C25 C26 Fe1 70.31(17) . . ?
C27 C26 Fe1 69.73(17) . . ?
C25 C26 H26A 126.1 . . ?
C27 C26 H26A 126.1 . . ?
Fe1 C26 H26A 126.1 . . ?
C26 C25 C24 109.0(3) . . ?
C26 C25 Fe1 69.03(17) . . ?
C24 C25 Fe1 72.33(17) . . ?
C26 C25 H25A 125.5 . . ?
C24 C25 H25A 125.5 . . ?
Fe1 C25 H25A 125.5 . . ?
C4 C3 C47 118.4(3) . . ?
C4 C3 C2 116.9(3) . . ?
C47 C3 C2 124.6(3) . . ?
C10 C9 C8 117.5(3) . . ?
C10 C9 C12 124.1(3) . . ?
C8 C9 C12 118.4(3) . . ?
C28 C27 C26 108.2(3) . . ?
C28 C27 Fe1 70.62(17) . . ?
C26 C27 Fe1 69.40(17) . . ?
C28 C27 H27A 125.9 . . ?
C26 C27 H27A 125.9 . . ?
Fe1 C27 H27A 125.9 . . ?
C12 C13 C48 121.2(3) . . ?
C12 C13 H13A 119.4 . . ?
C48 C13 H13A 119.4 . . ?
C13 C12 C9 120.2(3) . . ?
C13 C12 H12A 119.9 . . ?
C9 C12 H12A 119.9 . . ?
Si2 C35 H35A 109.5 . . ?
Si2 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si2 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N2 C24 C28 127.9(3) . . ?
N2 C24 C25 126.2(3) . . ?
C28 C24 C25 105.8(3) . . ?
N2 C24 Fe1 131.6(2) . . ?
C28 C24 Fe1 67.66(16) . . ?
C25 C24 Fe1 67.23(16) . . ?
N2 C24 Lu1 47.69(13) . . ?
C28 C24 Lu1 114.13(19) . . ?
C25 C24 Lu1 115.83(19) . . ?
Fe1 C24 Lu1 83.92(9) . . ?
C10 C11 N4 122.8(3) . . ?
C10 C11 H11A 118.6 . . ?
N4 C11 H11A 118.6 . . ?
Si2 C34 H34A 109.5 . . ?
Si2 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si2 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C18 C17 123.8(3) . . ?
N3 C18 H18A 118.1 . . ?
C17 C18 H18A 118.1 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C48 C49 C8 119.9(3) . . ?
C48 C49 H49A 120.0 . . ?
C8 C49 H49A 120.0 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C47 C46 C45 120.8(3) . . ?
C47 C46 H46A 119.6 . . ?
C45 C46 H46A 119.6 . . ?
C46 C45 C5 119.6(3) . . ?
C46 C45 H45A 120.2 . . ?
C5 C45 H45A 120.2 . . ?
C43 C44 C16 119.1(3) . . ?
C43 C44 H44A 120.4 . . ?
C16 C44 H44A 120.4 . . ?
C46 C47 C3 120.6(3) . . ?
C46 C47 H47A 119.7 . . ?
C3 C47 H47A 119.7 . . ?
C49 C48 C13 120.2(3) . . ?
C49 C48 H48A 119.9 . . ?
C13 C48 H48A 119.9 . . ?
C44 C43 C42 121.3(3) . . ?
C44 C43 H43A 119.4 . . ?
C42 C43 H43A 119.4 . . ?
C41 C42 C43 120.8(3) . . ?
C41 C42 H42A 119.6 . . ?
C43 C42 H42A 119.6 . . ?
C42 C41 C17 119.4(3) . . ?
C42 C41 H41A 120.3 . . ?
C17 C41 H41A 120.3 . . ?
C39 C37 C40 108.9(4) . . ?
C39 C37 C38 107.3(3) . . ?
C40 C37 C38 109.3(3) . . ?
C39 C37 Si2 109.7(3) . . ?
C40 C37 Si2 110.4(3) . . ?
C38 C37 Si2 111.2(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C2SA C1S C2SB 46.8(7) . . ?
C2SB C3S C2SA 56.1(8) . . ?
C2SB C3S C3S 157.2(17) . 2_655 ?
C2SA C3S C3S 144.2(16) . 2_655 ?
C2SB C3S H3SA 58.0 . . ?
C2SA C3S H3SA 100.9 . . ?
C3S C3S H3SA 100.9 2_655 . ?
C2SB C3S H3SB 78.8 . . ?
C2SA C3S H3SB 100.9 . . ?
C3S C3S H3SB 100.9 2_655 . ?
H3SA C3S H3SB 104.4 . . ?
C3S C2SA C1S 126.9(9) . . ?
C3S C2SA H2SA 105.6 . . ?
C1S C2SA H2SA 105.6 . . ?
C3S C2SA H2SB 105.6 . . ?
C1S C2SA H2SB 105.6 . . ?
H2SA C2SA H2SB 106.1 . . ?
C3S C2SB C1S 129.0(15) . . ?
C3S C2SB H2SC 105.0 . . ?
C1S C2SB H2SC 105.0 . . ?
C3S C2SB H2SD 105.0 . . ?
C1S C2SB H2SD 105.0 . . ?
H2SC C2SB H2SD 105.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 N2 2.204(2) . ?
Lu1 N1 2.227(2) . ?
Lu1 N5 2.241(2) . ?
Lu1 N4 2.433(2) . ?
Lu1 N3 2.438(2) . ?
Lu1 C24 2.891(3) . ?
Lu1 C19 2.903(3) . ?
Lu1 Fe1 3.3981(10) . ?
Fe1 C22 2.030(3) . ?
Fe1 C26 2.033(3) . ?
Fe1 C27 2.038(3) . ?
Fe1 C21 2.041(3) . ?
Fe1 C23 2.047(3) . ?
Fe1 C25 2.050(3) . ?
Fe1 C28 2.059(3) . ?
Fe1 C20 2.062(3) . ?
Fe1 C19 2.116(3) . ?
Fe1 C24 2.119(3) . ?
Si1 N1 1.727(2) . ?
Si1 C29 1.866(3) . ?
Si1 C36 1.885(3) . ?
Si1 C30 1.911(3) . ?
Si2 N2 1.725(2) . ?
Si2 C35 1.870(3) . ?
Si2 C34 1.871(4) . ?
Si2 C37 1.912(4) . ?
C1 N5 1.360(4) . ?
C1 C2 1.361(4) . ?
C1 H1A 0.9500 . ?
N3 C18 1.314(4) . ?
N3 C14 1.375(4) . ?
N4 C7 1.327(4) . ?
N4 C11 1.371(4) . ?
N2 C24 1.410(4) . ?
N1 C19 1.415(3) . ?
N5 C6 1.472(4) . ?
C19 C20 1.438(4) . ?
C19 C23 1.447(4) . ?
C23 C22 1.426(4) . ?
C23 H23A 1.0000 . ?
C14 C15 1.363(4) . ?
C14 H14A 0.9500 . ?
C17 C41 1.406(4) . ?
C17 C16 1.409(4) . ?
C17 C18 1.429(4) . ?
C21 C22 1.416(4) . ?
C21 C20 1.418(4) . ?
C21 H21A 1.0000 . ?
C20 H20A 1.0000 . ?
C22 H22A 1.0000 . ?
C6 C4 1.511(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.416(4) . ?
C7 H7A 0.9500 . ?
C5 C4 1.391(4) . ?
C5 C45 1.400(4) . ?
C5 H5A 0.9500 . ?
C30 C32 1.535(4) . ?
C30 C31 1.538(4) . ?
C30 C33 1.543(4) . ?
C8 C49 1.413(4) . ?
C8 C9 1.419(4) . ?
C15 C16 1.414(4) . ?
C15 H15A 0.9500 . ?
C16 C44 1.440(4) . ?
C2 C3 1.449(4) . ?
C2 H2A 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C10 C11 1.362(4) . ?
C10 C9 1.404(4) . ?
C10 H10A 0.9500 . ?
C28 C27 1.415(4) . ?
C28 C24 1.438(4) . ?
C28 H28A 1.0000 . ?
C4 C3 1.402(4) . ?
C26 C25 1.418(4) . ?
C26 C27 1.421(5) . ?
C26 H26A 1.0000 . ?
C25 C24 1.442(4) . ?
C25 H25A 1.0000 . ?
C3 C47 1.411(4) . ?
C9 C12 1.420(4) . ?
C27 H27A 1.0000 . ?
C13 C12 1.365(4) . ?
C13 C48 1.409(5) . ?
C13 H13A 0.9500 . ?
C12 H12A 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C11 H11A 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C18 H18A 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C49 C48 1.369(4) . ?
C49 H49A 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C46 C47 1.379(5) . ?
C46 C45 1.381(5) . ?
C46 H46A 0.9500 . ?
C45 H45A 0.9500 . ?
C44 C43 1.356(5) . ?
C44 H44A 0.9500 . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
C43 C42 1.416(5) . ?
C43 H43A 0.9500 . ?
C42 C41 1.369(5) . ?
C42 H42A 0.9500 . ?
C41 H41A 0.9500 . ?
C37 C39 1.537(5) . ?
C37 C40 1.537(6) . ?
C37 C38 1.541(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C1S C2SA 1.515(11) . ?
C1S C2SB 1.521(18) . ?
C3S C2SB 1.267(17) . ?
C3S C2SA 1.298(10) . ?
C3S C3S 1.349(13) 2_655 ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C2SA H2SA 0.9900 . ?
C2SA H2SB 0.9900 . ?
C2SB H2SC 0.9900 . ?
C2SB H2SD 0.9900 . ?
