# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tjm45
_database_code_depnum_ccdc_archive 'CCDC 1415191'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me5)2Lu]2(μ-η2:η2-N2)'
_chemical_name_common            1-Lu(A)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Lu2 N2'
_chemical_formula_weight         918.84

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6530(6)
_cell_length_b                   10.9963(6)
_cell_length_c                   16.6384(9)
_cell_angle_alpha                78.1853(6)
_cell_angle_beta                 78.1059(6)
_cell_angle_gamma                83.7548(6)
_cell_volume                     1862.31(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    4887
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      28.51

_exptl_crystal_description       'elongated plate'
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_F_000             912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.115
_exptl_absorpt_coefficient_mu    5.298
_shelx_estimated_absorpt_T_min   0.262
_shelx_estimated_absorpt_T_max   0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3637
_exptl_absorpt_correction_T_max  0.4924
_exptl_absorpt_process_details   'Bruker TWINABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8933
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.897
_diffrn_reflns_theta_max         28.889
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8933
_reflns_number_gt                7977
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2008.3-0, 2008'
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8933
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.12079(2) 0.36597(2) 0.25120(2) 0.01710(5) Uani 0.93 1 d . . P A 1
Lu2 Lu 0.42024(2) 0.06507(2) 0.24397(2) 0.02098(5) Uani 0.93 1 d . . P A 1
Lu3 Lu 0.0798(3) 0.4017(3) 0.2522(2) 0.0209(6) Uani 0.07 1 d . . P B 2
Lu4 Lu 0.4596(3) 0.0231(3) 0.2456(2) 0.0279(6) Uani 0.07 1 d . . P C 2
N1 N 0.2538(4) 0.2051(4) 0.2187(3) 0.0515(10) Uani 1 1 d . . . . .
N2 N 0.2812(4) 0.2191(4) 0.2769(3) 0.0512(9) Uani 1 1 d . . . . .
C1 C -0.0571(3) 0.2956(3) 0.3798(2) 0.0282(7) Uani 1 1 d . . . . .
C2 C 0.0588(3) 0.2759(3) 0.41108(19) 0.0300(8) Uani 1 1 d . . . . .
C3 C 0.1055(3) 0.3931(4) 0.40542(19) 0.0308(8) Uani 1 1 d . . . . .
C4 C 0.0159(3) 0.4872(3) 0.3745(2) 0.0302(7) Uani 1 1 d . . . . .
C5 C -0.0859(3) 0.4263(4) 0.3590(2) 0.0299(7) Uani 1 1 d . . . . .
C6 C -0.1417(4) 0.1973(4) 0.3756(2) 0.0412(9) Uani 1 1 d . . . . .
H6A H -0.1041 0.1150 0.3976 0.062 Uiso 1 1 calc R U . . .
H6B H -0.1489 0.2013 0.3173 0.062 Uiso 1 1 calc R U . . .
H6C H -0.2273 0.2115 0.4090 0.062 Uiso 1 1 calc R U . . .
C7 C 0.1173(4) 0.1523(4) 0.4503(2) 0.0418(9) Uani 1 1 d . . . . .
H7A H 0.0958 0.1427 0.5113 0.063 Uiso 1 1 calc R U . . .
H7B H 0.2109 0.1494 0.4321 0.063 Uiso 1 1 calc R U . . .
H7C H 0.0831 0.0847 0.4329 0.063 Uiso 1 1 calc R U . . .
C8 C 0.2205(4) 0.4192(4) 0.4373(2) 0.0430(10) Uani 1 1 d . . . . .
H8A H 0.2616 0.3405 0.4624 0.064 Uiso 1 1 calc R U . . .
H8B H 0.1926 0.4719 0.4795 0.064 Uiso 1 1 calc R U . . .
H8C H 0.2820 0.4621 0.3908 0.064 Uiso 1 1 calc R U . . .
C9 C 0.0201(4) 0.6233(4) 0.3738(2) 0.0388(9) Uani 1 1 d . . . . .
H9A H -0.0545 0.6693 0.3530 0.058 Uiso 1 1 calc R U . . .
H9B H 0.0993 0.6538 0.3372 0.058 Uiso 1 1 calc R U . . .
H9C H 0.0183 0.6358 0.4307 0.058 Uiso 1 1 calc R U . . .
C10 C -0.2141(4) 0.4844(4) 0.3420(2) 0.0389(9) Uani 1 1 d . . . . .
H10A H -0.2725 0.4908 0.3951 0.058 Uiso 1 1 calc R U . . .
H10B H -0.2501 0.4327 0.3121 0.058 Uiso 1 1 calc R U . . .
H10C H -0.2034 0.5677 0.3077 0.058 Uiso 1 1 calc R U . . .
C11 C -0.0045(3) 0.4835(3) 0.1318(2) 0.0264(7) Uani 1 1 d . . . . .
C12 C 0.0885(3) 0.3975(3) 0.09629(19) 0.0280(7) Uani 1 1 d . . . . .
C13 C 0.2117(3) 0.4376(3) 0.09264(19) 0.0303(8) Uani 1 1 d . . . . .
C14 C 0.1953(3) 0.5457(3) 0.1286(2) 0.0294(7) Uani 1 1 d . . . . .
C15 C 0.0610(3) 0.5753(3) 0.1505(2) 0.0279(7) Uani 1 1 d . . . . .
C16 C -0.1461(4) 0.4833(4) 0.1333(2) 0.0348(8) Uani 1 1 d . . . . .
H16A H -0.1911 0.5562 0.1546 0.052 Uiso 1 1 calc R U . . .
H16B H -0.1792 0.4073 0.1698 0.052 Uiso 1 1 calc R U . . .
H16C H -0.1602 0.4864 0.0766 0.052 Uiso 1 1 calc R U . . .
C17 C 0.0570(4) 0.2926(4) 0.0605(2) 0.0396(9) Uani 1 1 d . . . . .
H17A H 0.1368 0.2476 0.0381 0.059 Uiso 1 1 calc R U . . .
H17B H 0.0090 0.3261 0.0155 0.059 Uiso 1 1 calc R U . . .
H17C H 0.0046 0.2356 0.1045 0.059 Uiso 1 1 calc R U . . .
C18 C 0.3376(4) 0.3818(4) 0.0515(2) 0.0411(9) Uani 1 1 d . . . . .
H18A H 0.3377 0.2908 0.0649 0.062 Uiso 1 1 calc R U . . .
H18B H 0.4081 0.4084 0.0721 0.062 Uiso 1 1 calc R U . . .
H18C H 0.3492 0.4099 -0.0092 0.062 Uiso 1 1 calc R U . . .
C19 C 0.2983(4) 0.6249(4) 0.1344(3) 0.0407(9) Uani 1 1 d . . . . .
H19A H 0.2836 0.7095 0.1035 0.061 Uiso 1 1 calc R U . . .
H19B H 0.3826 0.5891 0.1104 0.061 Uiso 1 1 calc R U . . .
H19C H 0.2959 0.6277 0.1932 0.061 Uiso 1 1 calc R U . . .
C20 C 0.0034(4) 0.6989(3) 0.1706(2) 0.0383(9) Uani 1 1 d . . . . .
H20A H 0.0599 0.7322 0.1992 0.057 Uiso 1 1 calc R U . . .
H20B H -0.0811 0.6881 0.2071 0.057 Uiso 1 1 calc R U . . .
H20C H -0.0063 0.7571 0.1188 0.057 Uiso 1 1 calc R U . . .
C21 C 0.5683(4) 0.1550(4) 0.3188(3) 0.0417(10) Uani 1 1 d . . . . .
C22 C 0.5681(3) 0.2403(3) 0.2424(3) 0.0353(9) Uani 1 1 d . . . . .
C23 C 0.6311(3) 0.1817(3) 0.1768(3) 0.0330(8) Uani 1 1 d . . . . .
C24 C 0.6760(3) 0.0598(3) 0.2112(2) 0.0316(7) Uani 1 1 d . . . . .
C25 C 0.6374(3) 0.0417(4) 0.2999(2) 0.0372(9) Uani 1 1 d . . . . .
C26 C 0.5129(4) 0.1780(5) 0.4045(3) 0.0572(13) Uani 1 1 d . . . . .
H26A H 0.5389 0.1077 0.4458 0.086 Uiso 1 1 calc R U . . .
H26B H 0.4189 0.1868 0.4121 0.086 Uiso 1 1 calc R U . . .
H26C H 0.5445 0.2545 0.4121 0.086 Uiso 1 1 calc R U . . .
C27 C 0.5147(4) 0.3745(4) 0.2347(3) 0.0461(10) Uani 1 1 d . . . . .
H27A H 0.5828 0.4293 0.2048 0.069 Uiso 1 1 calc R U . . .
H27B H 0.4827 0.3937 0.2905 0.069 Uiso 1 1 calc R U . . .
H27C H 0.4441 0.3873 0.2036 0.069 Uiso 1 1 calc R U . . .
C28 C 0.6617(4) 0.2390(4) 0.0857(3) 0.0419(9) Uani 1 1 d . . . . .
H28A H 0.6245 0.3251 0.0773 0.063 Uiso 1 1 calc R U . . .
H28B H 0.6254 0.1911 0.0535 0.063 Uiso 1 1 calc R U . . .
H28C H 0.7552 0.2381 0.0670 0.063 Uiso 1 1 calc R U . . .
C29 C 0.7723(4) -0.0226(4) 0.1634(3) 0.0420(10) Uani 1 1 d . . . . .
H29A H 0.8590 0.0036 0.1587 0.063 Uiso 1 1 calc R U . . .
H29B H 0.7534 -0.0157 0.1074 0.063 Uiso 1 1 calc R U . . .
H29C H 0.7673 -0.1092 0.1929 0.063 Uiso 1 1 calc R U . . .
C30 C 0.6791(5) -0.0662(4) 0.3620(3) 0.0504(11) Uani 1 1 d . . . . .
H30A H 0.7316 -0.1281 0.3323 0.076 Uiso 1 1 calc R U . . .
H30B H 0.6032 -0.1043 0.3981 0.076 Uiso 1 1 calc R U . . .
H30C H 0.7299 -0.0370 0.3962 0.076 Uiso 1 1 calc R U . . .
C31 C 0.2357(3) -0.0830(3) 0.2621(2) 0.0284(7) Uani 1 1 d . . . . .
C32 C 0.3026(3) -0.0720(3) 0.1779(2) 0.0283(7) Uani 1 1 d . . . . .
C33 C 0.4276(3) -0.1312(3) 0.1776(2) 0.0338(8) Uani 1 1 d . . . . .
C34 C 0.4369(4) -0.1795(3) 0.2628(3) 0.0375(9) Uani 1 1 d . . . . .
C35 C 0.3197(4) -0.1477(3) 0.3140(2) 0.0356(9) Uani 1 1 d . . . . .
C36 C 0.0973(4) -0.0402(4) 0.2881(2) 0.0375(8) Uani 1 1 d . . . . .
H36A H 0.0432 -0.0827 0.2631 0.056 Uiso 1 1 calc R U . . .
H36B H 0.0857 0.0500 0.2689 0.056 Uiso 1 1 calc R U . . .
H36C H 0.0728 -0.0599 0.3492 0.056 Uiso 1 1 calc R U . . .
C37 C 0.2451(4) -0.0141(4) 0.1033(2) 0.0399(9) Uani 1 1 d . . . . .
H37A H 0.2043 -0.0775 0.0858 0.060 Uiso 1 1 calc R U . . .
H37B H 0.3126 0.0207 0.0575 0.060 Uiso 1 1 calc R U . . .
H37C H 0.1804 0.0524 0.1176 0.060 Uiso 1 1 calc R U . . .
C38 C 0.5232(4) -0.1506(5) 0.1009(3) 0.0535(12) Uani 1 1 d . . . . .
H38A H 0.4894 -0.2053 0.0720 0.080 Uiso 1 1 calc R U . . .
H38B H 0.6040 -0.1891 0.1170 0.080 Uiso 1 1 calc R U . . .
H38C H 0.5389 -0.0702 0.0636 0.080 Uiso 1 1 calc R U . . .
C39 C 0.5406(5) -0.2737(4) 0.2911(4) 0.0619(14) Uani 1 1 d . . . . .
H39A H 0.5206 -0.3572 0.2878 0.093 Uiso 1 1 calc R U . . .
H39B H 0.5449 -0.2709 0.3489 0.093 Uiso 1 1 calc R U . . .
H39C H 0.6236 -0.2540 0.2549 0.093 Uiso 1 1 calc R U . . .
C40 C 0.2867(5) -0.1849(4) 0.4079(3) 0.0532(12) Uani 1 1 d . . . . .
H40A H 0.2080 -0.1371 0.4291 0.080 Uiso 1 1 calc R U . . .
H40B H 0.3575 -0.1676 0.4324 0.080 Uiso 1 1 calc R U . . .
H40C H 0.2731 -0.2740 0.4232 0.080 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Cnt1 2.335 . ?
Lu1 Cnt2 2.334 . ?
Lu2 Cnt1 2.332 . ?
Lu2 Cnt1 2.320 . ?
Lu1 N1 2.227(4) . ?
Lu1 N2 2.265(4) . ?
Lu1 C14 2.593(3) . ?
Lu1 C1 2.595(3) . ?
Lu1 C13 2.604(3) . ?
Lu1 C3 2.614(3) . ?
Lu1 C2 2.614(3) . ?
Lu1 C12 2.618(3) . ?
Lu1 C5 2.655(3) . ?
Lu1 C15 2.656(3) . ?
Lu1 C11 2.658(3) . ?
Lu1 C4 2.661(3) . ?
Lu2 N2 2.205(4) . ?
Lu2 N1 2.267(4) . ?
Lu2 C21 2.582(3) . ?
Lu2 C32 2.590(3) . ?
Lu2 C33 2.605(3) . ?
Lu2 C22 2.611(3) . ?
Lu2 C31 2.618(3) . ?
Lu2 C35 2.625(3) . ?
Lu2 C34 2.634(4) . ?
Lu2 C25 2.635(3) . ?
Lu2 C23 2.635(3) . ?
Lu2 C24 2.662(3) . ?
N1 N2 1.111(5) . ?
C1 C2 1.414(5) . ?
C1 C5 1.423(5) . ?
C1 C6 1.502(5) . ?
C2 C3 1.410(5) . ?
C2 C7 1.511(5) . ?
C3 C4 1.421(6) . ?
C3 C8 1.506(5) . ?
C4 C5 1.426(5) . ?
C4 C9 1.500(5) . ?
C5 C10 1.499(5) . ?
C11 C15 1.406(5) . ?
C11 C12 1.417(5) . ?
C11 C16 1.503(5) . ?
C12 C13 1.415(5) . ?
C12 C17 1.498(5) . ?
C13 C14 1.416(5) . ?
C13 C18 1.503(5) . ?
C14 C15 1.420(5) . ?
C14 C19 1.503(5) . ?
C15 C20 1.503(5) . ?
C21 C22 1.416(6) . ?
C21 C25 1.435(6) . ?
C21 C26 1.488(6) . ?
C22 C23 1.396(5) . ?
C22 C27 1.512(6) . ?
C23 C24 1.419(5) . ?
C23 C28 1.499(5) . ?
C24 C25 1.425(5) . ?
C24 C29 1.504(6) . ?
C25 C30 1.499(6) . ?
C31 C35 1.407(5) . ?
C31 C32 1.423(4) . ?
C31 C36 1.500(5) . ?
C32 C33 1.416(5) . ?
C32 C37 1.492(5) . ?
C33 C34 1.428(6) . ?
C33 C38 1.497(5) . ?
C34 C35 1.412(6) . ?
C34 C39 1.510(6) . ?
C35 C40 1.509(5) . ?

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
Cnt1 Lu1 N1 123.8 . . ?
Cnt1 Lu1 N2 101.9 . . ?
Cnt2 Lu1 N1 102.3 . . ?
Cnt2 Lu1 N2 124.1 . . ?
Cnt1 Lu1 Cnt2 133.3 . . ?
Cnt3 Lu2 N1 119.4 . . ?
Cnt3 Lu2 N2 102.8 . . ?
Cnt4 Lu2 N1 103.2 . . ?
Cnt4 Lu2 N2 119.1 . . ?
Cnt3 Lu2 Cnt4 136.7 . . ?
N1 Lu1 N2 28.62(13) . . ?
N1 Lu1 C14 102.83(12) . . ?
N2 Lu1 C14 112.87(12) . . ?
N1 Lu1 C1 111.09(12) . . ?
N2 Lu1 C1 100.51(12) . . ?
C14 Lu1 C1 145.36(10) . . ?
N1 Lu1 C13 76.75(13) . . ?
N2 Lu1 C13 96.55(13) . . ?
C14 Lu1 C13 31.62(11) . . ?
C1 Lu1 C13 154.75(11) . . ?
N1 Lu1 C3 112.87(13) . . ?
N2 Lu1 C3 85.25(14) . . ?
C14 Lu1 C3 119.93(12) . . ?
C1 Lu1 C3 52.07(11) . . ?
C13 Lu1 C3 148.80(11) . . ?
N1 Lu1 C2 96.41(13) . . ?
N2 Lu1 C2 75.79(13) . . ?
C14 Lu1 C2 151.10(11) . . ?
C1 Lu1 C2 31.51(11) . . ?
C13 Lu1 C2 172.28(10) . . ?
C3 Lu1 C2 31.30(11) . . ?
N1 Lu1 C12 84.17(13) . . ?
N2 Lu1 C12 111.59(14) . . ?
C14 Lu1 C12 52.19(11) . . ?
C1 Lu1 C12 123.58(11) . . ?
C13 Lu1 C12 31.45(11) . . ?
C3 Lu1 C12 162.95(11) . . ?
C2 Lu1 C12 152.78(11) . . ?
N1 Lu1 C5 142.50(12) . . ?
N2 Lu1 C5 127.42(13) . . ?
C14 Lu1 C5 114.40(11) . . ?
C1 Lu1 C5 31.41(11) . . ?
C13 Lu1 C5 136.03(11) . . ?
C3 Lu1 C5 51.60(11) . . ?
C2 Lu1 C5 51.65(11) . . ?
C12 Lu1 C5 114.88(11) . . ?
N1 Lu1 C15 128.20(12) . . ?
N2 Lu1 C15 144.12(12) . . ?
C14 Lu1 C15 31.37(11) . . ?
C1 Lu1 C15 115.19(11) . . ?
C13 Lu1 C15 51.51(11) . . ?
C3 Lu1 C15 113.29(11) . . ?
C2 Lu1 C15 135.37(11) . . ?
C12 Lu1 C15 51.28(10) . . ?
C5 Lu1 C15 86.19(10) . . ?
N1 Lu1 C11 115.01(13) . . ?
N2 Lu1 C11 142.73(13) . . ?
C14 Lu1 C11 51.77(10) . . ?
C1 Lu1 C11 105.18(11) . . ?
C13 Lu1 C11 51.60(11) . . ?
C3 Lu1 C11 131.94(11) . . ?
C2 Lu1 C11 135.86(11) . . ?
C12 Lu1 C11 31.15(11) . . ?
C5 Lu1 C11 86.43(10) . . ?
C15 Lu1 C11 30.67(10) . . ?
N1 Lu1 C4 144.02(13) . . ?
N2 Lu1 C4 116.38(14) . . ?
C14 Lu1 C4 102.41(11) . . ?
C1 Lu1 C4 51.93(11) . . ?
C13 Lu1 C4 133.50(11) . . ?
C3 Lu1 C4 31.23(12) . . ?
C2 Lu1 C4 51.65(11) . . ?
C12 Lu1 C4 131.76(11) . . ?
C5 Lu1 C4 31.11(10) . . ?
C15 Lu1 C4 85.15(11) . . ?
C11 Lu1 C4 100.73(10) . . ?
N2 Lu2 N1 28.73(14) . . ?
N2 Lu2 C21 85.02(15) . . ?
N1 Lu2 C21 110.05(14) . . ?
N2 Lu2 C32 106.73(14) . . ?
N1 Lu2 C32 82.78(13) . . ?
C21 Lu2 C32 166.94(13) . . ?
N2 Lu2 C33 138.37(13) . . ?
N1 Lu2 C33 113.28(14) . . ?
C21 Lu2 C33 136.26(13) . . ?
C32 Lu2 C33 31.64(12) . . ?
N2 Lu2 C22 77.05(13) . . ?
N1 Lu2 C22 92.17(13) . . ?
C21 Lu2 C22 31.64(13) . . ?
C32 Lu2 C22 155.34(12) . . ?
C33 Lu2 C22 139.13(12) . . ?
N2 Lu2 C31 91.72(13) . . ?
N1 Lu2 C31 79.01(12) . . ?
C21 Lu2 C31 145.70(12) . . ?
C32 Lu2 C31 31.71(10) . . ?
C33 Lu2 C31 52.41(11) . . ?
C22 Lu2 C31 168.34(11) . . ?
N2 Lu2 C35 109.10(13) . . ?
N1 Lu2 C35 106.45(13) . . ?
C21 Lu2 C35 119.40(13) . . ?
C32 Lu2 C35 51.95(11) . . ?
C33 Lu2 C35 52.24(12) . . ?
C22 Lu2 C35 150.99(12) . . ?
C31 Lu2 C35 31.12(11) . . ?
N2 Lu2 C34 139.99(13) . . ?
N1 Lu2 C34 129.99(12) . . ?
C21 Lu2 C34 115.33(13) . . ?
C32 Lu2 C34 51.86(11) . . ?
C33 Lu2 C34 31.62(12) . . ?
C22 Lu2 C34 137.83(11) . . ?
C31 Lu2 C34 51.61(11) . . ?
C35 Lu2 C34 31.15(12) . . ?
N2 Lu2 C25 116.72(14) . . ?
N1 Lu2 C25 141.52(13) . . ?
C21 Lu2 C25 31.90(13) . . ?
C32 Lu2 C25 135.57(12) . . ?
C33 Lu2 C25 104.35(12) . . ?
C22 Lu2 C25 52.12(12) . . ?
C31 Lu2 C25 133.65(12) . . ?
C35 Lu2 C25 102.60(12) . . ?
C34 Lu2 C25 87.00(12) . . ?
N2 Lu2 C23 102.01(13) . . ?
N1 Lu2 C23 106.12(12) . . ?
C21 Lu2 C23 51.94(13) . . ?
C32 Lu2 C23 128.25(11) . . ?
C33 Lu2 C23 108.69(11) . . ?
C22 Lu2 C23 30.87(12) . . ?
C31 Lu2 C23 159.63(12) . . ?
C35 Lu2 C23 146.99(11) . . ?
C34 Lu2 C23 117.75(12) . . ?
C25 Lu2 C23 51.86(12) . . ?
N2 Lu2 C24 128.35(13) . . ?
N1 Lu2 C24 137.19(12) . . ?
C21 Lu2 C24 51.91(12) . . ?
C32 Lu2 C24 120.12(11) . . ?
C33 Lu2 C24 90.61(11) . . ?
C22 Lu2 C24 51.29(12) . . ?
C31 Lu2 C24 139.82(11) . . ?
C35 Lu2 C24 116.14(12) . . ?
C34 Lu2 C24 88.99(11) . . ?
C25 Lu2 C24 31.21(12) . . ?
C23 Lu2 C24 31.08(11) . . ?
N2 N1 Lu1 77.6(4) . . ?
N2 N1 Lu2 72.5(3) . . ?
Lu1 N1 Lu2 150.0(2) . . ?
N1 N2 Lu2 78.7(4) . . ?
N1 N2 Lu1 73.8(3) . . ?
Lu2 N2 Lu1 152.4(2) . . ?
C2 C1 C5 108.0(3) . . ?
C2 C1 C6 126.6(3) . . ?
C5 C1 C6 125.2(3) . . ?
C2 C1 Lu1 74.97(18) . . ?
C5 C1 Lu1 76.61(18) . . ?
C6 C1 Lu1 118.5(2) . . ?
C3 C2 C1 108.1(3) . . ?
C3 C2 C7 125.4(3) . . ?
C1 C2 C7 126.3(3) . . ?
C3 C2 Lu1 74.34(17) . . ?
C1 C2 Lu1 73.52(18) . . ?
C7 C2 Lu1 121.8(2) . . ?
C2 C3 C4 108.6(3) . . ?
C2 C3 C8 127.1(4) . . ?
C4 C3 C8 123.8(4) . . ?
C2 C3 Lu1 74.36(18) . . ?
C4 C3 Lu1 76.24(19) . . ?
C8 C3 Lu1 122.2(2) . . ?
C3 C4 C5 107.4(3) . . ?
C3 C4 C9 124.2(3) . . ?
C5 C4 C9 127.6(4) . . ?
C3 C4 Lu1 72.53(19) . . ?
C5 C4 Lu1 74.19(19) . . ?
C9 C4 Lu1 126.8(2) . . ?
C1 C5 C4 107.9(3) . . ?
C1 C5 C10 123.8(3) . . ?
C4 C5 C10 127.1(4) . . ?
C1 C5 Lu1 71.98(19) . . ?
C4 C5 Lu1 74.70(19) . . ?
C10 C5 Lu1 128.7(2) . . ?
C15 C11 C12 107.9(3) . . ?
C15 C11 C16 128.0(3) . . ?
C12 C11 C16 123.3(3) . . ?
C15 C11 Lu1 74.60(19) . . ?
C12 C11 Lu1 72.88(18) . . ?
C16 C11 Lu1 126.3(2) . . ?
C13 C12 C11 108.0(3) . . ?
C13 C12 C17 127.5(3) . . ?
C11 C12 C17 124.2(3) . . ?
C13 C12 Lu1 73.71(18) . . ?
C11 C12 Lu1 75.98(18) . . ?
C17 C12 Lu1 121.8(2) . . ?
C12 C13 C14 108.1(3) . . ?
C12 C13 C18 126.1(3) . . ?
C14 C13 C18 125.6(3) . . ?
C12 C13 Lu1 74.85(18) . . ?
C14 C13 Lu1 73.76(18) . . ?
C18 C13 Lu1 121.2(2) . . ?
C13 C14 C15 107.4(3) . . ?
C13 C14 C19 127.3(3) . . ?
C15 C14 C19 125.0(3) . . ?
C13 C14 Lu1 74.62(18) . . ?
C15 C14 Lu1 76.79(18) . . ?
C19 C14 Lu1 119.8(2) . . ?
C11 C15 C14 108.5(3) . . ?
C11 C15 C20 126.3(3) . . ?
C14 C15 C20 123.8(3) . . ?
C11 C15 Lu1 74.73(18) . . ?
C14 C15 Lu1 71.84(18) . . ?
C20 C15 Lu1 130.1(2) . . ?
C22 C21 C25 107.9(4) . . ?
C22 C21 C26 127.1(4) . . ?
C25 C21 C26 124.9(4) . . ?
C22 C21 Lu2 75.30(19) . . ?
C25 C21 Lu2 76.07(19) . . ?
C26 C21 Lu2 116.9(3) . . ?
C23 C22 C21 108.7(3) . . ?
C23 C22 C27 126.2(4) . . ?
C21 C22 C27 125.1(4) . . ?
C23 C22 Lu2 75.52(18) . . ?
C21 C22 Lu2 73.06(19) . . ?
C27 C22 Lu2 120.2(2) . . ?
C22 C23 C24 108.3(3) . . ?
C22 C23 C28 127.2(4) . . ?
C24 C23 C28 124.1(4) . . ?
C22 C23 Lu2 73.61(19) . . ?
C24 C23 Lu2 75.52(19) . . ?
C28 C23 Lu2 122.4(2) . . ?
C23 C24 C25 108.2(3) . . ?
C23 C24 C29 124.4(4) . . ?
C25 C24 C29 126.0(4) . . ?
C23 C24 Lu2 73.40(19) . . ?
C25 C24 Lu2 73.3(2) . . ?
C29 C24 Lu2 129.7(2) . . ?
C24 C25 C21 106.8(3) . . ?
C24 C25 C30 126.4(4) . . ?
C21 C25 C30 126.1(4) . . ?
C24 C25 Lu2 75.5(2) . . ?
C21 C25 Lu2 72.03(19) . . ?
C30 C25 Lu2 125.3(3) . . ?
C35 C31 C32 107.6(3) . . ?
C35 C31 C36 127.5(3) . . ?
C32 C31 C36 124.7(3) . . ?
C35 C31 Lu2 74.70(18) . . ?
C32 C31 Lu2 73.04(17) . . ?
C36 C31 Lu2 121.3(2) . . ?
C33 C32 C31 108.6(3) . . ?
C33 C32 C37 126.8(3) . . ?
C31 C32 C37 124.5(3) . . ?
C33 C32 Lu2 74.76(19) . . ?
C31 C32 Lu2 75.25(18) . . ?
C37 C32 Lu2 119.2(2) . . ?
C32 C33 C34 106.9(3) . . ?
C32 C33 C38 125.1(4) . . ?
C34 C33 C38 127.7(4) . . ?
C32 C33 Lu2 73.60(19) . . ?
C34 C33 Lu2 75.3(2) . . ?
C38 C33 Lu2 122.0(2) . . ?
C35 C34 C33 108.4(3) . . ?
C35 C34 C39 125.3(4) . . ?
C33 C34 C39 124.9(4) . . ?
C35 C34 Lu2 74.1(2) . . ?
C33 C34 Lu2 73.1(2) . . ?
C39 C34 Lu2 129.8(3) . . ?
C31 C35 C34 108.4(3) . . ?
C31 C35 C40 125.6(4) . . ?
C34 C35 C40 125.8(4) . . ?
C31 C35 Lu2 74.18(19) . . ?
C34 C35 Lu2 74.78(19) . . ?
C40 C35 Lu2 120.6(3) . . ?

_refine_diff_density_max         1.234
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.106

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef9
_database_code_depnum_ccdc_archive 'CCDC 1415192'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me5)2Lu]2(μ-η2:η2-N2)'
_chemical_name_common            1-Lu(B)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Lu2 N2'
_chemical_formula_weight         918.84

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.4028(16)
_cell_length_b                   14.4028(16)
_cell_length_c                   19.526(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4050.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9986
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.58

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.107
_exptl_absorpt_coefficient_mu    4.872
_shelx_estimated_absorpt_T_min   0.252
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3701
_exptl_absorpt_correction_T_max  0.7823
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38645
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.000
_diffrn_reflns_theta_max         27.131
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4478
_reflns_number_gt                3999
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2010.9-1, 2010'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.107 x 0.111 x 0.390 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.
The APEX2 program package was used to determine the unit-cell parameters and
for data collection (25 sec/frame scan time for a sphere of diffraction data).
The raw frame data was processed using SAINT and SADABS to yield the reflection
data file.  Subsequent calculations were carried out using the SHELXTL program.
The diffraction symmetry was 4/mmm and the systematic absences were consistent
with the tetragonal space group P-42(1)c that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix
least-squares techniques.  The analytical scattering factors for neutral atoms
were used throughout the analysis.  Hydrogen atoms were included using a riding
model.  The molecule was located about a two-fold rotation axis. The lutetium
atom was disordered approximately 84% (Lu1), 16% (Lu2).
Metric data involving the lutetium atom was referenced to the major component
Lu(1).  Carbon atoms C(16)-C(20) were disordered and included using multiple
components, partial site-occupancy-factors and isotropic thermal parameters.

At convergence, wR2 = 0.0911 and Goof = 1.145 for 219 variables refined against
4478 data (0.80), R1 = 0.0325 for those 3999 data with I > 2.0sigma(I).  The
absolute structure was assigned by refinement of the Flack parameter.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0551P)²+1.1575P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1667 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.026(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4478
_refine_ls_number_parameters     219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.1488(3) 0.46603(6) 1.15550(4) 0.0285(4) Uani 0.835(12) 1 d . . P A .
Lu2 Lu 0.1867(12) 0.4575(4) 1.1530(2) 0.0304(15) Uani 0.165(12) 1 d . . P . .
N1 N 0.0087(6) 0.5404(5) 1.1531(4) 0.0532(18) Uani 1 1 d . . . . .
C1 C 0.2967(7) 0.5620(7) 1.1108(4) 0.044(2) Uani 1 1 d . . . . .
C2 C 0.2959(7) 0.4793(7) 1.0709(4) 0.048(2) Uani 1 1 d . . . . .
C3 C 0.2147(8) 0.4799(7) 1.0313(5) 0.054(3) Uani 1 1 d . . . . .
C4 C 0.1662(7) 0.5636(7) 1.0435(5) 0.045(2) Uani 1 1 d . . . . .
C5 C 0.2171(7) 0.6127(6) 1.0956(5) 0.043(2) Uani 1 1 d . . . . .
C6 C 0.3730(7) 0.5976(8) 1.1560(6) 0.060(2) Uani 1 1 d . . . . .
H6A H 0.3470 0.6170 1.2001 0.090 Uiso 1 1 calc R U . . .
H6B H 0.4031 0.6509 1.1340 0.090 Uiso 1 1 calc R U . . .
H6C H 0.4189 0.5484 1.1635 0.090 Uiso 1 1 calc R U . . .
C7 C 0.3762(8) 0.4127(9) 1.0597(6) 0.071(4) Uani 1 1 d . . . . .
H7A H 0.4294 0.4467 1.0410 0.106 Uiso 1 1 calc R U . . .
H7B H 0.3573 0.3641 1.0274 0.106 Uiso 1 1 calc R U . . .
H7C H 0.3936 0.3843 1.1035 0.106 Uiso 1 1 calc R U . . .
C8 C 0.1892(10) 0.4055(9) 0.9796(6) 0.073(4) Uani 1 1 d . . . . .
H8A H 0.2004 0.3441 0.9996 0.110 Uiso 1 1 calc R U . . .
H8B H 0.2272 0.4130 0.9384 0.110 Uiso 1 1 calc R U . . .
H8C H 0.1234 0.4113 0.9676 0.110 Uiso 1 1 calc R U . . .
C9 C 0.0864(8) 0.6014(9) 1.0062(6) 0.063(3) Uani 1 1 d . . . . .
H9A H 0.0901 0.5828 0.9580 0.095 Uiso 1 1 calc R U . . .
H9B H 0.0867 0.6693 1.0094 0.095 Uiso 1 1 calc R U . . .
H9C H 0.0288 0.5772 1.0262 0.095 Uiso 1 1 calc R U . . .
C10 C 0.1933(8) 0.7079(6) 1.1229(6) 0.055(3) Uani 1 1 d . . . . .
H10A H 0.2499 0.7455 1.1259 0.083 Uiso 1 1 calc R U . . .
H10B H 0.1654 0.7020 1.1684 0.083 Uiso 1 1 calc R U . . .
H10C H 0.1491 0.7381 1.0919 0.083 Uiso 1 1 calc R U . . .
C11 C 0.1097(7) 0.3639(7) 1.2606(5) 0.052(2) Uani 1 1 d . . . . .
C12 C 0.1381(8) 0.3017(6) 1.2092(6) 0.055(3) Uani 1 1 d . . . . .
C13 C 0.2337(8) 0.3123(7) 1.2002(6) 0.058(3) Uani 1 1 d . . . . .
C14 C 0.2638(7) 0.3832(7) 1.2448(5) 0.045(2) Uani 1 1 d . . . . .
C15 C 0.1886(7) 0.4155(7) 1.2819(5) 0.051(2) Uani 1 1 d . . . . .
C16 C 0.0124(15) 0.3522(18) 1.2785(13) 0.051(5) Uiso 0.5 1 d . . P A 1
H16A H 0.0029 0.2902 1.2979 0.076 Uiso 0.5 1 calc R U P A 1
H16B H -0.0259 0.3592 1.2374 0.076 Uiso 0.5 1 calc R U P A 1
H16C H -0.0054 0.3992 1.3123 0.076 Uiso 0.5 1 calc R U P A 1
C17 C 0.0924(17) 0.2289(17) 1.1565(15) 0.059(6) Uiso 0.5 1 d . . P A 1
H17A H 0.0441 0.2601 1.1296 0.089 Uiso 0.5 1 calc R U P A 1
H17B H 0.0647 0.1773 1.1822 0.089 Uiso 0.5 1 calc R U P A 1
H17C H 0.1404 0.2049 1.1257 0.089 Uiso 0.5 1 calc R U P A 1
C18 C 0.273(2) 0.241(2) 1.1441(15) 0.073(8) Uiso 0.5 1 d . . P A 1
H18A H 0.3410 0.2440 1.1433 0.109 Uiso 0.5 1 calc R U P A 1
H18B H 0.2485 0.2571 1.0988 0.109 Uiso 0.5 1 calc R U P A 1
H18C H 0.2536 0.1776 1.1560 0.109 Uiso 0.5 1 calc R U P A 1
C19 C 0.3713(15) 0.3905(16) 1.2497(12) 0.050(5) Uiso 0.5 1 d . . P A 1
H19A H 0.3915 0.4505 1.2313 0.075 Uiso 0.5 1 calc R U P A 1
H19B H 0.3997 0.3402 1.2231 0.075 Uiso 0.5 1 calc R U P A 1
H19C H 0.3904 0.3855 1.2977 0.075 Uiso 0.5 1 calc R U P A 1
C20 C 0.2112(18) 0.4837(15) 1.3400(13) 0.051(5) Uiso 0.5 1 d . . P A 1
H20A H 0.2787 0.4888 1.3452 0.076 Uiso 0.5 1 calc R U P A 1
H20B H 0.1840 0.4611 1.3829 0.076 Uiso 0.5 1 calc R U P A 1
H20C H 0.1853 0.5449 1.3291 0.076 Uiso 0.5 1 calc R U P A 1
C16B C 0.0191(16) 0.3782(17) 1.3007(14) 0.053(6) Uiso 0.5 1 d . . P A 2
H16D H 0.0060 0.3227 1.3282 0.079 Uiso 0.5 1 calc R U P A 2
H16E H -0.0321 0.3889 1.2686 0.079 Uiso 0.5 1 calc R U P A 2
H16F H 0.0256 0.4320 1.3311 0.079 Uiso 0.5 1 calc R U P A 2
C17B C 0.0686(17) 0.2364(17) 1.1812(13) 0.057(6) Uiso 0.5 1 d . . P A 2
H17D H 0.0147 0.2339 1.2118 0.085 Uiso 0.5 1 calc R U P A 2
H17E H 0.0961 0.1744 1.1774 0.085 Uiso 0.5 1 calc R U P A 2
H17F H 0.0488 0.2576 1.1357 0.085 Uiso 0.5 1 calc R U P A 2
C18B C 0.3014(18) 0.2502(17) 1.1631(13) 0.057(6) Uiso 0.5 1 d . . P A 2
H18D H 0.3650 0.2709 1.1725 0.085 Uiso 0.5 1 calc R U P A 2
H18E H 0.2897 0.2533 1.1137 0.085 Uiso 0.5 1 calc R U P A 2
H18F H 0.2937 0.1861 1.1789 0.085 Uiso 0.5 1 calc R U P A 2
C19B C 0.3606(15) 0.4190(16) 1.2682(11) 0.046(5) Uiso 0.5 1 d . . P A 2
H19D H 0.3721 0.4804 1.2484 0.070 Uiso 0.5 1 calc R U P A 2
H19E H 0.4088 0.3757 1.2528 0.070 Uiso 0.5 1 calc R U P A 2
H19F H 0.3620 0.4234 1.3183 0.070 Uiso 0.5 1 calc R U P A 2
C20B C 0.177(2) 0.4782(18) 1.3433(15) 0.062(7) Uiso 0.5 1 d . . P A 2
H20D H 0.1686 0.5423 1.3278 0.093 Uiso 0.5 1 calc R U P A 2
H20E H 0.2331 0.4745 1.3719 0.093 Uiso 0.5 1 calc R U P A 2
H20F H 0.1232 0.4585 1.3699 0.093 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Cnt1 2.352 . ?
Lu1 Cnt2 2.349 . ?
Lu1 N1 2.271(9) 2_565 ?
Lu1 N1 2.286(9) . ?
Lu1 C11 2.587(9) . ?
Lu1 C12 2.593(9) . ?
Lu1 C5 2.607(9) . ?
Lu1 C4 2.611(9) . ?
Lu1 C3 2.612(9) . ?
Lu1 C15 2.636(9) . ?
Lu1 C13 2.675(10) . ?
Lu1 C14 2.684(9) . ?
Lu1 C1 2.684(10) . ?
Lu1 C2 2.693(10) . ?
N1 N1 1.190(16) 2_565 ?
N1 Lu1 2.271(9) 2_565 ?
C1 C5 1.390(13) . ?
C1 C2 1.423(13) . ?
C1 C6 1.501(14) . ?
C2 C3 1.402(15) . ?
C2 C7 1.518(14) . ?
C3 C4 1.414(14) . ?
C3 C8 1.518(14) . ?
C4 C5 1.439(14) . ?
C4 C9 1.466(15) . ?
C5 C10 1.511(13) . ?
C11 C12 1.405(16) . ?
C11 C15 1.420(14) . ?
C11 C16 1.45(2) . ?
C11 C16B 1.54(3) . ?
C12 C13 1.396(16) . ?
C12 C17B 1.48(3) . ?
C12 C17 1.61(3) . ?
C13 C14 1.410(15) . ?
C13 C18B 1.51(3) . ?
C13 C18 1.61(3) . ?
C14 C15 1.383(15) . ?
C14 C19 1.55(2) . ?
C14 C19B 1.56(2) . ?
C15 C20B 1.51(3) . ?
C15 C20 1.54(3) . ?

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
Cnt1 Lu1 N1 104.9 . . ?
Cnt1 Lu1 N1 123.4 2_565 . ?
Cnt2 Lu1 N1 122.5 . . ?
Cnt2 Lu1 N1 102.7 2_565 . ?
Cnt1 Lu1 Cnt2 132.1 . . ?
N1 Lu1 N1 30.3(4) 2_565 . ?
N1 Lu1 C11 77.0(3) 2_565 . ?
N1 Lu1 C11 95.2(3) . . ?
N1 Lu1 C12 84.9(3) 2_565 . ?
N1 Lu1 C12 112.6(3) . . ?
C11 Lu1 C12 31.5(4) . . ?
N1 Lu1 C5 113.6(3) 2_565 . ?
N1 Lu1 C5 86.8(3) . . ?
C11 Lu1 C5 154.0(3) . . ?
C12 Lu1 C5 160.6(4) . . ?
N1 Lu1 C4 95.7(3) 2_565 . ?
N1 Lu1 C4 79.3(3) . . ?
C11 Lu1 C4 172.4(3) . . ?
C12 Lu1 C4 146.7(3) . . ?
C5 Lu1 C4 32.0(3) . . ?
N1 Lu1 C3 110.3(3) 2_565 . ?
N1 Lu1 C3 105.4(3) . . ?
C11 Lu1 C3 149.2(3) . . ?
C12 Lu1 C3 117.9(4) . . ?
C5 Lu1 C3 52.0(3) . . ?
C4 Lu1 C3 31.4(3) . . ?
N1 Lu1 C15 103.0(3) 2_565 . ?
N1 Lu1 C15 109.9(3) . . ?
C11 Lu1 C15 31.5(3) . . ?
C12 Lu1 C15 51.8(3) . . ?
C5 Lu1 C15 124.2(3) . . ?
C4 Lu1 C15 155.7(3) . . ?
C3 Lu1 C15 144.2(4) . . ?
N1 Lu1 C13 115.4(3) 2_565 . ?
N1 Lu1 C13 143.0(3) . . ?
C11 Lu1 C13 51.0(3) . . ?
C12 Lu1 C13 30.7(3) . . ?
C5 Lu1 C13 130.1(4) . . ?
C4 Lu1 C13 132.4(4) . . ?
C3 Lu1 C13 101.5(4) . . ?
C15 Lu1 C13 50.7(4) . . ?
N1 Lu1 C14 127.7(3) 2_565 . ?
N1 Lu1 C14 140.1(3) . . ?
C11 Lu1 C14 50.7(3) . . ?
C12 Lu1 C14 50.8(3) . . ?
C5 Lu1 C14 114.7(3) . . ?
C4 Lu1 C14 136.4(3) . . ?
C3 Lu1 C14 114.4(4) . . ?
C15 Lu1 C14 30.1(3) . . ?
C13 Lu1 C14 30.5(3) . . ?
N1 Lu1 C1 143.8(3) 2_565 . ?
N1 Lu1 C1 116.9(3) . . ?
C11 Lu1 C1 136.3(3) . . ?
C12 Lu1 C1 130.4(3) . . ?
C5 Lu1 C1 30.4(3) . . ?
C4 Lu1 C1 51.3(3) . . ?
C3 Lu1 C1 51.0(3) . . ?
C15 Lu1 C1 105.9(3) . . ?
C13 Lu1 C1 99.8(3) . . ?
C14 Lu1 C1 87.2(3) . . ?
N1 Lu1 C2 140.9(3) 2_565 . ?
N1 Lu1 C2 130.5(3) . . ?
C11 Lu1 C2 134.3(3) . . ?
C12 Lu1 C2 111.1(3) . . ?
C5 Lu1 C2 51.0(3) . . ?
C4 Lu1 C2 51.2(3) . . ?
C3 Lu1 C2 30.6(3) . . ?
C15 Lu1 C2 115.0(3) . . ?
C13 Lu1 C2 84.2(3) . . ?
C14 Lu1 C2 86.8(3) . . ?
C1 Lu1 C2 30.7(3) . . ?
N1 N1 Lu1 75.6(8) 2_565 2_565 ?
N1 N1 Lu1 74.2(7) 2_565 . ?
Lu1 N1 Lu1 149.6(4) 2_565 . ?
C5 C1 C2 108.4(8) . . ?
C5 C1 C6 123.4(9) . . ?
C2 C1 C6 127.9(9) . . ?
C5 C1 Lu1 71.7(5) . . ?
C2 C1 Lu1 75.0(5) . . ?
C6 C1 Lu1 124.5(6) . . ?
C3 C2 C1 107.6(9) . . ?
C3 C2 C7 124.0(9) . . ?
C1 C2 C7 127.0(10) . . ?
C3 C2 Lu1 71.5(6) . . ?
C1 C2 Lu1 74.3(5) . . ?
C7 C2 Lu1 130.0(7) . . ?
C2 C3 C4 108.9(9) . . ?
C2 C3 C8 124.4(10) . . ?
C4 C3 C8 126.5(11) . . ?
C2 C3 Lu1 77.9(5) . . ?
C4 C3 Lu1 74.3(5) . . ?
C8 C3 Lu1 118.3(8) . . ?
C3 C4 C5 106.6(8) . . ?
C3 C4 C9 128.3(10) . . ?
C5 C4 C9 124.7(10) . . ?
C3 C4 Lu1 74.3(5) . . ?
C5 C4 Lu1 73.8(5) . . ?
C9 C4 Lu1 122.7(7) . . ?
C1 C5 C4 108.3(8) . . ?
C1 C5 C10 126.1(10) . . ?
C4 C5 C10 125.3(9) . . ?
C1 C5 Lu1 77.9(5) . . ?
C4 C5 Lu1 74.2(5) . . ?
C10 C5 Lu1 119.4(6) . . ?
C12 C11 C15 108.0(9) . . ?
C12 C11 C16 112.2(14) . . ?
C15 C11 C16 139.6(15) . . ?
C12 C11 C16B 134.2(13) . . ?
C15 C11 C16B 117.4(14) . . ?
C12 C11 Lu1 74.5(5) . . ?
C15 C11 Lu1 76.1(5) . . ?
C16 C11 Lu1 117.9(11) . . ?
C16B C11 Lu1 120.9(10) . . ?
C13 C12 C11 108.0(9) . . ?
C13 C12 C17B 133.6(15) . . ?
C11 C12 C17B 118.2(14) . . ?
C13 C12 C17 113.1(14) . . ?
C11 C12 C17 138.7(13) . . ?
C13 C12 Lu1 77.9(6) . . ?
C11 C12 Lu1 74.0(5) . . ?
C17B C12 Lu1 118.1(11) . . ?
C17 C12 Lu1 111.1(11) . . ?
C12 C13 C14 107.7(10) . . ?
C12 C13 C18B 129.3(14) . . ?
C14 C13 C18B 121.8(14) . . ?
C12 C13 C18 111.4(14) . . ?
C14 C13 C18 141.0(15) . . ?
C12 C13 Lu1 71.4(5) . . ?
C14 C13 Lu1 75.1(5) . . ?
C18B C13 Lu1 129.0(11) . . ?
C18 C13 Lu1 118.0(12) . . ?
C15 C14 C13 109.0(9) . . ?
C15 C14 C19 136.4(13) . . ?
C13 C14 C19 113.1(12) . . ?
C15 C14 C19B 115.9(12) . . ?
C13 C14 C19B 134.2(12) . . ?
C15 C14 Lu1 73.0(5) . . ?
C13 C14 Lu1 74.4(5) . . ?
C19 C14 Lu1 128.6(10) . . ?
C19B C14 Lu1 126.7(10) . . ?
C14 C15 C11 107.3(9) . . ?
C14 C15 C20B 134.4(15) . . ?
C11 C15 C20B 117.4(15) . . ?
C14 C15 C20 115.8(13) . . ?
C11 C15 C20 136.1(14) . . ?
C14 C15 Lu1 76.9(6) . . ?
C11 C15 Lu1 72.3(5) . . ?
C20B C15 Lu1 123.7(11) . . ?
C20 C15 Lu1 124.1(10) . . ?

_refine_diff_density_max         1.275
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.159

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef11
_database_code_depnum_ccdc_archive 'CCDC 1415193'
_audit_update_record             
;
2016-02-01 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Lu2 N2'
_chemical_formula_weight         918.84

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.3199(19)
_cell_length_b                   14.3199(19)
_cell_length_c                   19.597(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4018.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.85

_exptl_crystal_description       needle_rod
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.083
_exptl_absorpt_coefficient_mu    4.911
_shelx_estimated_absorpt_T_min   0.398
_shelx_estimated_absorpt_T_max   0.686
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2759
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48692
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.011
_diffrn_reflns_theta_max         29.195
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5242
_reflns_number_gt                4919
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_max     0.944
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2010.9-1, 2010'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.083 x 0.096 x 0.230 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.
The APEX2 program package was used to determine the unit-cell parameters and
for data collection (25 sec/frame scan time for a sphere of diffraction data).
The raw frame data was processed using SAINT and SADABS to yield the reflection
data file.  Subsequent calculations were carried out using the SHELXTL program.
The diffraction symmetry was 4/mmm and the systematic absences were consistent
with the tetragonal space group P-42(1)c that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix
least-squares techniques.  The analytical scattering factors for neutral atoms
were used throughout the analysis.  Hydrogen atoms were included using a riding
model.  The molecule was located about a two-fold rotation axis.  The lutetium 
atom was disordered approximately 92% (Lu1), 8% (Lu2).
Metric data involving the lutetium atom was referenced to the major component Lu(1).
Carbon atoms C(16)-C(20) were disordered and included using multiple components,
partial site-occupancy-factors and isotropic thermal parameters.

At convergence, wR2 = 0.0660 and Goof = 1.082 for 218 variables refined against
5242 data (0.73), R1 = 0.0254 for those 4919 data with I > 2.0sigma(I).  The
absolute structure was assigned by refinement of the Flack parameter.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2070 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.005(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5242
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.85097(3) 0.53355(2) -0.15528(2) 0.02392(9) Uani 0.92 1 d . . P A .
Lu2 Lu 0.8142(3) 0.5388(3) -0.1528(3) 0.0262(9) Uani 0.08 1 d . . P . .
N1 N 0.9901(3) 0.4581(3) -0.1538(3) 0.0409(10) Uani 1 1 d . . . . .
C1 C 0.7043(4) 0.4380(4) -0.1109(3) 0.0348(12) Uani 1 1 d . . . . .
C2 C 0.7063(4) 0.5211(5) -0.0706(3) 0.0422(14) Uani 1 1 d . . . . .
C3 C 0.7882(5) 0.5199(5) -0.0309(3) 0.0429(15) Uani 1 1 d . . . . .
C4 C 0.8356(4) 0.4341(4) -0.0439(3) 0.0371(13) Uani 1 1 d . . . . .
C5 C 0.7839(4) 0.3857(4) -0.0947(3) 0.0340(12) Uani 1 1 d . . . . .
C6 C 0.6249(5) 0.4033(5) -0.1539(4) 0.0514(15) Uani 1 1 d . . . . .
H6A H 0.6489 0.3830 -0.1984 0.077 Uiso 1 1 calc R U . . .
H6B H 0.5794 0.4536 -0.1605 0.077 Uiso 1 1 calc R U . . .
H6C H 0.5946 0.3505 -0.1311 0.077 Uiso 1 1 calc R U . . .
C7 C 0.6245(6) 0.5872(6) -0.0587(4) 0.061(2) Uani 1 1 d . . . . .
H7A H 0.5767 0.5556 -0.0314 0.092 Uiso 1 1 calc R U . . .
H7B H 0.5979 0.6059 -0.1027 0.092 Uiso 1 1 calc R U . . .
H7C H 0.6465 0.6428 -0.0343 0.092 Uiso 1 1 calc R U . . .
C8 C 0.8146(7) 0.5942(6) 0.0206(4) 0.067(2) Uani 1 1 d . . . . .
H8A H 0.7811 0.6522 0.0101 0.101 Uiso 1 1 calc R U . . .
H8B H 0.8820 0.6055 0.0184 0.101 Uiso 1 1 calc R U . . .
H8C H 0.7976 0.5731 0.0665 0.101 Uiso 1 1 calc R U . . .
C9 C 0.9174(5) 0.3959(7) -0.0073(4) 0.057(2) Uani 1 1 d . . . . .
H9A H 0.9295 0.4336 0.0335 0.086 Uiso 1 1 calc R U . . .
H9B H 0.9721 0.3977 -0.0373 0.086 Uiso 1 1 calc R U . . .
H9C H 0.9047 0.3313 0.0062 0.086 Uiso 1 1 calc R U . . .
C10 C 0.8069(5) 0.2898(4) -0.1225(4) 0.0496(17) Uani 1 1 d . . . . .
H10A H 0.8045 0.2440 -0.0854 0.074 Uiso 1 1 calc R U . . .
H10B H 0.8697 0.2905 -0.1423 0.074 Uiso 1 1 calc R U . . .
H10C H 0.7614 0.2729 -0.1577 0.074 Uiso 1 1 calc R U . . .
C11 C 0.8913(5) 0.6366(5) -0.2613(4) 0.0504(17) Uani 1 1 d . . . . .
C12 C 0.8612(5) 0.6976(4) -0.2104(4) 0.0524(18) Uani 1 1 d . . . . .
C13 C 0.7656(5) 0.6848(5) -0.2025(4) 0.0549(18) Uani 1 1 d . . . . .
C14 C 0.7358(5) 0.6141(5) -0.2455(4) 0.0436(15) Uani 1 1 d . . . . .
C15 C 0.8117(5) 0.5818(5) -0.2819(4) 0.0502(17) Uani 1 1 d . . . . .
C16 C 0.9895(9) 0.6493(11) -0.2797(8) 0.042(3) Uiso 0.5 1 d . . P A 1
H16A H 0.9945 0.6961 -0.3160 0.063 Uiso 0.5 1 calc R U P A 1
H16B H 1.0153 0.5899 -0.2957 0.063 Uiso 0.5 1 calc R U P A 1
H16C H 1.0245 0.6705 -0.2396 0.063 Uiso 0.5 1 calc R U P A 1
C17 C 0.9073(10) 0.7740(10) -0.1600(9) 0.049(3) Uiso 0.5 1 d . . P A 1
H17A H 0.9711 0.7550 -0.1486 0.073 Uiso 0.5 1 calc R U P A 1
H17B H 0.8700 0.7784 -0.1182 0.073 Uiso 0.5 1 calc R U P A 1
H17C H 0.9086 0.8349 -0.1828 0.073 Uiso 0.5 1 calc R U P A 1
C18 C 0.7264(15) 0.7574(15) -0.1433(10) 0.071(5) Uiso 0.5 1 d . . P A 1
H18A H 0.7126 0.8180 -0.1642 0.107 Uiso 0.5 1 calc R U P A 1
H18B H 0.7740 0.7653 -0.1079 0.107 Uiso 0.5 1 calc R U P A 1
H18C H 0.6694 0.7318 -0.1229 0.107 Uiso 0.5 1 calc R U P A 1
C19 C 0.6295(9) 0.6048(10) -0.2495(7) 0.040(3) Uiso 0.5 1 d . . P A 1
H19A H 0.6070 0.5681 -0.2107 0.060 Uiso 0.5 1 calc R U P A 1
H19B H 0.6123 0.5734 -0.2922 0.060 Uiso 0.5 1 calc R U P A 1
H19C H 0.6011 0.6671 -0.2483 0.060 Uiso 0.5 1 calc R U P A 1
C20 C 0.7919(10) 0.5136(9) -0.3393(7) 0.039(3) Uiso 0.5 1 d . . P A 1
H20A H 0.7265 0.4938 -0.3371 0.059 Uiso 0.5 1 calc R U P A 1
H20B H 0.8326 0.4590 -0.3346 0.059 Uiso 0.5 1 calc R U P A 1
H20C H 0.8039 0.5440 -0.3832 0.059 Uiso 0.5 1 calc R U P A 1
C16B C 0.9811(9) 0.6175(10) -0.3069(7) 0.042(3) Uiso 0.5 1 d . . P A 2
H16D H 0.9806 0.6594 -0.3464 0.063 Uiso 0.5 1 calc R U P A 2
H16E H 0.9805 0.5525 -0.3226 0.063 Uiso 0.5 1 calc R U P A 2
H16F H 1.0375 0.6287 -0.2798 0.063 Uiso 0.5 1 calc R U P A 2
C17B C 0.9373(12) 0.7607(13) -0.1881(10) 0.062(4) Uiso 0.5 1 d . . P A 2
H17D H 0.9931 0.7493 -0.2159 0.093 Uiso 0.5 1 calc R U P A 2
H17E H 0.9518 0.7488 -0.1400 0.093 Uiso 0.5 1 calc R U P A 2
H17F H 0.9175 0.8257 -0.1936 0.093 Uiso 0.5 1 calc R U P A 2
C18B C 0.6976(12) 0.7474(12) -0.1650(9) 0.054(4) Uiso 0.5 1 d . . P A 2
H18D H 0.6363 0.7170 -0.1630 0.081 Uiso 0.5 1 calc R U P A 2
H18E H 0.6921 0.8070 -0.1892 0.081 Uiso 0.5 1 calc R U P A 2
H18F H 0.7204 0.7586 -0.1186 0.081 Uiso 0.5 1 calc R U P A 2
C19B C 0.6407(11) 0.5779(11) -0.2700(8) 0.047(3) Uiso 0.5 1 d . . P A 2
H19D H 0.5955 0.5818 -0.2325 0.071 Uiso 0.5 1 calc R U P A 2
H19E H 0.6469 0.5128 -0.2847 0.071 Uiso 0.5 1 calc R U P A 2
H19F H 0.6190 0.6161 -0.3083 0.071 Uiso 0.5 1 calc R U P A 2
C20B C 0.8360(15) 0.5259(13) -0.3430(10) 0.069(5) Uiso 0.5 1 d . . P A 2
H20D H 0.7988 0.4685 -0.3435 0.104 Uiso 0.5 1 calc R U P A 2
H20E H 0.9025 0.5101 -0.3418 0.104 Uiso 0.5 1 calc R U P A 2
H20F H 0.8226 0.5623 -0.3842 0.104 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Cnt1 2.336 . ?
Lu1 Cnt2 2.351 . ?
Lu1 N1 2.267(5) . ?
Lu1 N1 2.279(5) 2_765 ?
Lu1 C12 2.589(6) . ?
Lu1 C3 2.604(6) . ?
Lu1 C5 2.610(5) . ?
Lu1 C11 2.614(6) . ?
Lu1 C4 2.615(6) . ?
Lu1 C15 2.636(7) . ?
Lu1 C13 2.653(6) . ?
Lu1 C1 2.654(6) . ?
Lu1 C2 2.660(6) . ?
Lu1 C14 2.679(6) . ?
N1 N1 1.233(10) 2_765 ?
N1 Lu1 2.279(5) 2_765 ?
C1 C5 1.401(8) . ?
C1 C2 1.427(9) . ?
C1 C6 1.500(8) . ?
C2 C3 1.408(9) . ?
C2 C7 1.524(9) . ?
C3 C4 1.426(10) . ?
C3 C8 1.514(9) . ?
C4 C5 1.421(9) . ?
C4 C9 1.479(9) . ?
C5 C10 1.512(8) . ?
C11 C12 1.394(11) . ?
C11 C15 1.441(10) . ?
C11 C16 1.464(15) . ?
C11 C16B 1.589(16) . ?
C12 C13 1.390(11) . ?
C12 C17B 1.482(18) . ?
C12 C17 1.614(16) . ?
C13 C14 1.385(11) . ?
C13 C18B 1.514(17) . ?
C13 C18 1.66(2) . ?
C14 C15 1.380(11) . ?
C14 C19 1.530(15) . ?
C14 C19B 1.533(16) . ?
C15 C20B 1.48(2) . ?
C15 C20 1.516(16) . ?

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
Cnt1 Lu1 N1 104.2 . . ?
Cnt1 Lu1 N1 123.3 . 2_765 ?
Cnt2 Lu1 N1 122.0 . . ?
Cnt2 Lu1 N1 101.8 . 2_765 ?
Cnt1 Lu1 Cnt2 133.1 . . ?
N1 Lu1 N1 31.5(2) . 2_765 ?
N1 Lu1 C12 112.8(2) . . ?
N1 Lu1 C12 84.3(2) 2_765 . ?
N1 Lu1 C3 104.8(2) . . ?
N1 Lu1 C3 109.7(2) 2_765 . ?
C12 Lu1 C3 118.5(2) . . ?
N1 Lu1 C5 86.04(18) . . ?
N1 Lu1 C5 113.83(18) 2_765 . ?
C12 Lu1 C5 161.1(2) . . ?
C3 Lu1 C5 52.2(2) . . ?
N1 Lu1 C11 94.9(2) . . ?
N1 Lu1 C11 76.1(2) 2_765 . ?
C12 Lu1 C11 31.1(2) . . ?
C3 Lu1 C11 149.6(2) . . ?
C5 Lu1 C11 154.3(2) . . ?
N1 Lu1 C4 78.69(19) . . ?
N1 Lu1 C4 95.86(19) 2_765 . ?
C12 Lu1 C4 147.9(2) . . ?
C3 Lu1 C4 31.7(2) . . ?
C5 Lu1 C4 31.6(2) . . ?
C11 Lu1 C4 171.8(2) . . ?
N1 Lu1 C15 108.9(2) . . ?
N1 Lu1 C15 102.2(2) 2_765 . ?
C12 Lu1 C15 51.8(2) . . ?
C3 Lu1 C15 145.8(2) . . ?
C5 Lu1 C15 124.2(2) . . ?
C11 Lu1 C15 31.9(2) . . ?
C4 Lu1 C15 155.5(2) . . ?
N1 Lu1 C13 143.0(2) . . ?
N1 Lu1 C13 114.9(2) 2_765 . ?
C12 Lu1 C13 30.7(2) . . ?
C3 Lu1 C13 103.2(2) . . ?
C5 Lu1 C13 130.6(2) . . ?
C11 Lu1 C13 50.5(2) . . ?
C4 Lu1 C13 134.2(2) . . ?
C15 Lu1 C13 50.2(3) . . ?
N1 Lu1 C1 116.49(18) . . ?
N1 Lu1 C1 144.43(19) 2_765 . ?
C12 Lu1 C1 130.5(2) . . ?
C3 Lu1 C1 51.79(19) . . ?
C5 Lu1 C1 30.86(18) . . ?
C11 Lu1 C1 136.6(2) . . ?
C4 Lu1 C1 51.61(19) . . ?
C15 Lu1 C1 106.0(2) . . ?
C13 Lu1 C1 99.8(2) . . ?
N1 Lu1 C2 130.15(19) . . ?
N1 Lu1 C2 140.7(2) 2_765 . ?
C12 Lu1 C2 111.4(2) . . ?
C3 Lu1 C2 31.0(2) . . ?
C5 Lu1 C2 51.36(18) . . ?
C11 Lu1 C2 134.9(2) . . ?
C4 Lu1 C2 51.50(19) . . ?
C15 Lu1 C2 116.0(2) . . ?
C13 Lu1 C2 85.0(2) . . ?
C1 Lu1 C2 31.16(19) . . ?
N1 Lu1 C14 139.0(2) . . ?
N1 Lu1 C14 126.9(2) 2_765 . ?
C12 Lu1 C14 50.9(2) . . ?
C3 Lu1 C14 115.9(2) . . ?
C5 Lu1 C14 115.0(2) . . ?
C11 Lu1 C14 50.8(2) . . ?
C4 Lu1 C14 137.2(2) . . ?
C15 Lu1 C14 30.1(2) . . ?
C13 Lu1 C14 30.1(2) . . ?
C1 Lu1 C14 87.19(19) . . ?
C2 Lu1 C14 87.8(2) . . ?
N1 N1 Lu1 74.8(4) 2_765 . ?
N1 N1 Lu1 73.7(4) 2_765 2_765 ?
Lu1 N1 Lu1 148.5(2) . 2_765 ?
C5 C1 C2 107.7(5) . . ?
C5 C1 C6 124.5(6) . . ?
C2 C1 C6 127.0(6) . . ?
C5 C1 Lu1 72.9(3) . . ?
C2 C1 Lu1 74.7(3) . . ?
C6 C1 Lu1 125.9(4) . . ?
C3 C2 C1 108.2(6) . . ?
C3 C2 C7 124.2(6) . . ?
C1 C2 C7 126.0(6) . . ?
C3 C2 Lu1 72.3(3) . . ?
C1 C2 Lu1 74.2(3) . . ?
C7 C2 Lu1 130.7(4) . . ?
C2 C3 C4 107.9(6) . . ?
C2 C3 C8 124.6(7) . . ?
C4 C3 C8 127.3(7) . . ?
C2 C3 Lu1 76.7(3) . . ?
C4 C3 Lu1 74.6(3) . . ?
C8 C3 Lu1 119.0(5) . . ?
C5 C4 C3 107.3(5) . . ?
C5 C4 C9 124.9(6) . . ?
C3 C4 C9 127.5(7) . . ?
C5 C4 Lu1 74.0(3) . . ?
C3 C4 Lu1 73.7(3) . . ?
C9 C4 Lu1 122.7(4) . . ?
C1 C5 C4 108.7(5) . . ?
C1 C5 C10 125.6(6) . . ?
C4 C5 C10 125.5(6) . . ?
C1 C5 Lu1 76.3(3) . . ?
C4 C5 Lu1 74.4(3) . . ?
C10 C5 Lu1 119.5(4) . . ?
C12 C11 C15 107.3(6) . . ?
C12 C11 C16 113.3(9) . . ?
C15 C11 C16 139.4(9) . . ?
C12 C11 C16B 139.5(8) . . ?
C15 C11 C16B 112.9(8) . . ?
C12 C11 Lu1 73.5(4) . . ?
C15 C11 Lu1 74.9(4) . . ?
C16 C11 Lu1 118.6(6) . . ?
C16B C11 Lu1 121.9(6) . . ?
C13 C12 C11 107.5(6) . . ?
C13 C12 C17B 140.5(10) . . ?
C11 C12 C17B 111.5(10) . . ?
C13 C12 C17 115.1(9) . . ?
C11 C12 C17 137.4(8) . . ?
C13 C12 Lu1 77.2(4) . . ?
C11 C12 Lu1 75.4(3) . . ?
C17B C12 Lu1 118.2(8) . . ?
C17 C12 Lu1 112.5(7) . . ?
C14 C13 C12 109.4(7) . . ?
C14 C13 C18B 122.0(10) . . ?
C12 C13 C18B 127.6(10) . . ?
C14 C13 C18 141.3(10) . . ?
C12 C13 C18 109.2(10) . . ?
C14 C13 Lu1 76.0(4) . . ?
C12 C13 Lu1 72.1(4) . . ?
C18B C13 Lu1 127.6(8) . . ?
C18 C13 Lu1 115.1(8) . . ?
C15 C14 C13 108.4(6) . . ?
C15 C14 C19 136.7(9) . . ?
C13 C14 C19 113.7(8) . . ?
C15 C14 C19B 115.1(8) . . ?
C13 C14 C19B 135.3(9) . . ?
C15 C14 Lu1 73.2(4) . . ?
C13 C14 Lu1 73.9(4) . . ?
C19 C14 Lu1 127.5(6) . . ?
C19B C14 Lu1 127.4(7) . . ?
C14 C15 C11 107.2(7) . . ?
C14 C15 C20B 141.6(11) . . ?
C11 C15 C20B 109.5(11) . . ?
C14 C15 C20 116.8(8) . . ?
C11 C15 C20 134.9(9) . . ?
C14 C15 Lu1 76.7(4) . . ?
C11 C15 Lu1 73.2(4) . . ?
C20B C15 Lu1 124.7(8) . . ?
C20 C15 Lu1 124.7(6) . . ?

_refine_diff_density_max         1.084
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.132

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef1
_database_code_depnum_ccdc_archive 'CCDC 1415194'
_audit_update_record             
;
2016-02-01 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Lu2 N2'
_chemical_formula_weight         918.84

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.317(3)
_cell_length_b                   14.317(3)
_cell_length_c                   19.639(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4026(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9319
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      27.97

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.109
_exptl_absorpt_coefficient_mu    4.902
_shelx_estimated_absorpt_T_min   0.400
_shelx_estimated_absorpt_T_max   0.617
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3310
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42682
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.012
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4430
_reflns_number_gt                4204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2010.9-1, 2010'
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1812 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.002(8)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4430
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.14925(3) 0.46664(2) 1.15516(2) 0.02633(11) Uani 0.96 1 d . . P A 1
Lu2 Lu 0.1855(9) 0.4620(6) 1.1537(6) 0.032(3) Uiso 0.04 1 d . . P B 2
N1 N 0.0092(4) 0.5423(4) 1.1539(3) 0.0391(13) Uani 1 1 d . . . . .
C1 C 0.2949(5) 0.5629(6) 1.1104(4) 0.0358(16) Uani 1 1 d . . . . .
C2 C 0.2938(5) 0.4790(6) 1.0710(4) 0.0395(17) Uani 1 1 d . . . . .
C3 C 0.2119(6) 0.4804(6) 1.0317(4) 0.0433(19) Uani 1 1 d . . . . .
C4 C 0.1639(6) 0.5665(6) 1.0444(4) 0.0380(17) Uani 1 1 d . . . . .
C5 C 0.2154(5) 0.6149(5) 1.0953(4) 0.0359(16) Uani 1 1 d . . . . .
C6 C 0.3737(5) 0.5974(6) 1.1546(5) 0.0510(19) Uani 1 1 d . . . . .
H6A H 0.3483 0.6227 1.1972 0.076 Uiso 1 1 calc R U . . .
H6B H 0.4081 0.6465 1.1306 0.076 Uiso 1 1 calc R U . . .
H6C H 0.4160 0.5455 1.1650 0.076 Uiso 1 1 calc R U . . .
C7 C 0.3751(6) 0.4144(7) 1.0587(5) 0.056(2) Uani 1 1 d . . . . .
H7A H 0.4262 0.4493 1.0374 0.084 Uiso 1 1 calc R U . . .
H7B H 0.3556 0.3635 1.0286 0.084 Uiso 1 1 calc R U . . .
H7C H 0.3964 0.3885 1.1022 0.084 Uiso 1 1 calc R U . . .
C8 C 0.1850(8) 0.4072(8) 0.9789(5) 0.064(3) Uani 1 1 d . . . . .
H8A H 0.1929 0.3447 0.9984 0.096 Uiso 1 1 calc R U . . .
H8B H 0.2251 0.4138 0.9388 0.096 Uiso 1 1 calc R U . . .
H8C H 0.1196 0.4161 0.9656 0.096 Uiso 1 1 calc R U . . .
C9 C 0.0818(7) 0.6034(8) 1.0071(5) 0.057(3) Uani 1 1 d . . . . .
H9A H 0.0723 0.5671 0.9654 0.085 Uiso 1 1 calc R U . . .
H9B H 0.0926 0.6690 0.9953 0.085 Uiso 1 1 calc R U . . .
H9C H 0.0262 0.5986 1.0360 0.085 Uiso 1 1 calc R U . . .
C10 C 0.1923(7) 0.7111(6) 1.1226(5) 0.050(2) Uani 1 1 d . . . . .
H10A H 0.1934 0.7564 1.0852 0.076 Uiso 1 1 calc R U . . .
H10B H 0.2386 0.7289 1.1570 0.076 Uiso 1 1 calc R U . . .
H10C H 0.1300 0.7102 1.1432 0.076 Uiso 1 1 calc R U . . .
C11 C 0.1079(6) 0.3642(6) 1.2611(4) 0.048(2) Uani 1 1 d . . . . .
C12 C 0.1374(7) 0.3033(5) 1.2099(5) 0.051(2) Uani 1 1 d . . . . .
C13 C 0.2337(6) 0.3150(6) 1.2009(5) 0.050(2) Uani 1 1 d . . . . .
C14 C 0.2638(6) 0.3863(6) 1.2441(5) 0.045(2) Uani 1 1 d . . . . .
C15 C 0.1880(6) 0.4185(6) 1.2817(5) 0.047(2) Uani 1 1 d . . . . .
C16 C 0.0101(12) 0.3517(14) 1.2807(10) 0.043(4) Uiso 0.5 1 d . . P A 1
H16A H -0.0127 0.4086 1.3029 0.064 Uiso 0.5 1 calc R U P A 1
H16B H 0.0049 0.2990 1.3123 0.064 Uiso 0.5 1 calc R U P A 1
H16C H -0.0275 0.3391 1.2400 0.064 Uiso 0.5 1 calc R U P A 1
C17 C 0.0936(15) 0.2274(14) 1.1585(12) 0.056(5) Uiso 0.5 1 d . . P A 1
H17A H 0.1373 0.2162 1.1210 0.083 Uiso 0.5 1 calc R U P A 1
H17B H 0.0344 0.2510 1.1403 0.083 Uiso 0.5 1 calc R U P A 1
H17C H 0.0825 0.1689 1.1831 0.083 Uiso 0.5 1 calc R U P A 1
C18 C 0.2741(18) 0.2435(18) 1.1397(12) 0.071(7) Uiso 0.5 1 d . . P A 1
H18A H 0.2413 0.2564 1.0969 0.106 Uiso 0.5 1 calc R U P A 1
H18B H 0.2633 0.1784 1.1531 0.106 Uiso 0.5 1 calc R U P A 1
H18C H 0.3412 0.2540 1.1335 0.106 Uiso 0.5 1 calc R U P A 1
C19 C 0.3710(14) 0.3964(15) 1.2472(11) 0.051(5) Uiso 0.5 1 d . . P A 1
H19A H 0.4003 0.3414 1.2265 0.076 Uiso 0.5 1 calc R U P A 1
H19B H 0.3909 0.4016 1.2948 0.076 Uiso 0.5 1 calc R U P A 1
H19C H 0.3900 0.4525 1.2222 0.076 Uiso 0.5 1 calc R U P A 1
C20 C 0.2098(14) 0.4880(13) 1.3389(10) 0.044(4) Uiso 0.5 1 d . . P A 1
H20A H 0.1701 0.5434 1.3339 0.065 Uiso 0.5 1 calc R U P A 1
H20B H 0.2756 0.5065 1.3364 0.065 Uiso 0.5 1 calc R U P A 1
H20C H 0.1976 0.4586 1.3831 0.065 Uiso 0.5 1 calc R U P A 1
C16A C 0.0200(13) 0.3815(13) 1.3050(10) 0.044(4) Uiso 0.5 1 d . . P A 2
H16D H 0.0382 0.4116 1.3478 0.067 Uiso 0.5 1 calc R U P A 2
H16E H -0.0104 0.3217 1.3149 0.067 Uiso 0.5 1 calc R U P A 2
H16F H -0.0234 0.4220 1.2802 0.067 Uiso 0.5 1 calc R U P A 2
C17A C 0.0652(15) 0.2374(15) 1.1828(11) 0.053(5) Uiso 0.5 1 d . . P A 2
H17D H 0.0903 0.1737 1.1828 0.080 Uiso 0.5 1 calc R U P A 2
H17E H 0.0485 0.2554 1.1363 0.080 Uiso 0.5 1 calc R U P A 2
H17F H 0.0095 0.2399 1.2118 0.080 Uiso 0.5 1 calc R U P A 2
C18A C 0.2992(13) 0.2520(12) 1.1639(9) 0.042(4) Uiso 0.5 1 d . . P A 2
H18D H 0.3308 0.2110 1.1965 0.063 Uiso 0.5 1 calc R U P A 2
H18E H 0.3457 0.2895 1.1396 0.063 Uiso 0.5 1 calc R U P A 2
H18F H 0.2641 0.2140 1.1311 0.063 Uiso 0.5 1 calc R U P A 2
C19A C 0.3617(13) 0.4213(13) 1.2685(9) 0.041(4) Uiso 0.5 1 d . . P A 2
H19D H 0.4070 0.4145 1.2314 0.062 Uiso 0.5 1 calc R U P A 2
H19E H 0.3821 0.3842 1.3077 0.062 Uiso 0.5 1 calc R U P A 2
H19F H 0.3574 0.4872 1.2816 0.062 Uiso 0.5 1 calc R U P A 2
C20A C 0.173(2) 0.4754(18) 1.3413(13) 0.066(6) Uiso 0.5 1 d . . P A 2
H20D H 0.1093 0.5007 1.3404 0.100 Uiso 0.5 1 calc R U P A 2
H20E H 0.2179 0.5270 1.3417 0.100 Uiso 0.5 1 calc R U P A 2
H20F H 0.1812 0.4372 1.3823 0.100 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 Cnt1 2.330 . ?
Lu1 Cnt1 2.338 . ?
Lu1 N1 2.272(6) 2_565 ?
Lu1 N1 2.279(6) . ?
Lu1 C12 2.579(8) . ?
Lu1 C3 2.593(7) . ?
Lu1 C5 2.605(7) . ?
Lu1 C4 2.612(7) . ?
Lu1 C11 2.613(8) . ?
Lu1 C15 2.637(9) . ?
Lu1 C13 2.642(8) . ?
Lu1 C1 2.649(8) . ?
Lu1 C2 2.655(7) . ?
Lu1 C14 2.658(8) . ?
N1 N1 1.239(12) 2_565 ?
N1 Lu1 2.272(6) 2_565 ?
C1 C5 1.391(11) . ?
C1 C2 1.430(11) . ?
C1 C6 1.508(10) . ?
C2 C3 1.404(11) . ?
C2 C7 1.505(11) . ?
C3 C4 1.432(12) . ?
C3 C8 1.523(12) . ?
C4 C5 1.423(11) . ?
C4 C9 1.482(12) . ?
C5 C10 1.515(11) . ?
C11 C12 1.397(13) . ?
C11 C15 1.443(13) . ?
C11 C16 1.46(2) . ?
C11 C16A 1.55(2) . ?
C12 C13 1.399(13) . ?
C12 C17A 1.50(2) . ?
C12 C17 1.61(2) . ?
C13 C14 1.395(14) . ?
C13 C18A 1.492(19) . ?
C13 C18 1.68(2) . ?
C14 C15 1.391(13) . ?
C14 C19 1.54(2) . ?
C14 C19A 1.56(2) . ?
C15 C20A 1.44(3) . ?
C15 C20 1.53(2) . ?

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


Cnt1 Lu1 N1 104.2 . . ?
Cnt1 Lu1 N1 123.3 2_565 . ?
Cnt2 Lu1 N1 121.6 . . ?
Cnt2 Lu1 N1 101.3 2_565 . ?
Cnt1 Lu1 Cnt2 133.6 . . ?
N1 Lu1 N1 31.6(3) 2_565 . ?
N1 Lu1 C12 83.6(3) 2_565 . ?
N1 Lu1 C12 112.2(3) . . ?
N1 Lu1 C3 109.8(3) 2_565 . ?
N1 Lu1 C3 104.9(3) . . ?
C12 Lu1 C3 118.8(3) . . ?
N1 Lu1 C5 113.8(2) 2_565 . ?
N1 Lu1 C5 85.9(2) . . ?
C12 Lu1 C5 161.9(3) . . ?
C3 Lu1 C5 52.4(3) . . ?
N1 Lu1 C4 95.9(2) 2_565 . ?
N1 Lu1 C4 78.6(2) . . ?
C12 Lu1 C4 148.1(3) . . ?
C3 Lu1 C4 31.9(3) . . ?
C5 Lu1 C4 31.7(3) . . ?
N1 Lu1 C11 75.6(2) 2_565 . ?
N1 Lu1 C11 94.4(3) . . ?
C12 Lu1 C11 31.2(3) . . ?
C3 Lu1 C11 149.9(3) . . ?
C5 Lu1 C11 154.0(3) . . ?
C4 Lu1 C11 171.3(3) . . ?
N1 Lu1 C15 101.9(3) 2_565 . ?
N1 Lu1 C15 108.6(3) . . ?
C12 Lu1 C15 52.0(3) . . ?
C3 Lu1 C15 145.9(3) . . ?
C5 Lu1 C15 124.2(3) . . ?
C4 Lu1 C15 155.6(3) . . ?
C11 Lu1 C15 31.9(3) . . ?
N1 Lu1 C13 114.5(3) 2_565 . ?
N1 Lu1 C13 142.8(3) . . ?
C12 Lu1 C13 31.1(3) . . ?
C3 Lu1 C13 102.9(3) . . ?
C5 Lu1 C13 131.0(3) . . ?
C4 Lu1 C13 134.1(3) . . ?
C11 Lu1 C13 51.1(3) . . ?
C15 Lu1 C13 50.9(3) . . ?
N1 Lu1 C1 144.2(2) 2_565 . ?
N1 Lu1 C1 116.2(2) . . ?
C12 Lu1 C1 131.4(3) . . ?
C3 Lu1 C1 51.5(3) . . ?
C5 Lu1 C1 30.7(2) . . ?
C4 Lu1 C1 51.4(2) . . ?
C11 Lu1 C1 137.3(3) . . ?
C15 Lu1 C1 106.4(3) . . ?
C13 Lu1 C1 100.4(3) . . ?
N1 Lu1 C2 140.8(2) 2_565 . ?
N1 Lu1 C2 130.3(2) . . ?
C12 Lu1 C2 111.8(3) . . ?
C3 Lu1 C2 31.0(2) . . ?
C5 Lu1 C2 51.8(2) . . ?
C4 Lu1 C2 51.8(2) . . ?
C11 Lu1 C2 135.2(2) . . ?
C15 Lu1 C2 116.1(3) . . ?
C13 Lu1 C2 84.8(3) . . ?
C1 Lu1 C2 31.3(2) . . ?
N1 Lu1 C14 126.8(3) 2_565 . ?
N1 Lu1 C14 139.1(3) . . ?
C12 Lu1 C14 51.3(3) . . ?
C3 Lu1 C14 115.7(3) . . ?
C5 Lu1 C14 115.2(3) . . ?
C4 Lu1 C14 137.3(3) . . ?
C11 Lu1 C14 51.2(3) . . ?
C15 Lu1 C14 30.5(3) . . ?
C13 Lu1 C14 30.5(3) . . ?
C1 Lu1 C14 87.6(2) . . ?
C2 Lu1 C14 87.6(3) . . ?
N1 N1 Lu1 74.5(5) 2_565 2_565 ?
N1 N1 Lu1 73.9(5) 2_565 . ?
Lu1 N1 Lu1 148.4(3) 2_565 . ?
C5 C1 C2 109.0(7) . . ?
C5 C1 C6 124.0(8) . . ?
C2 C1 C6 126.6(7) . . ?
C5 C1 Lu1 72.9(4) . . ?
C2 C1 Lu1 74.6(4) . . ?
C6 C1 Lu1 124.6(5) . . ?
C3 C2 C1 107.1(7) . . ?
C3 C2 C7 124.6(8) . . ?
C1 C2 C7 126.4(7) . . ?
C3 C2 Lu1 72.1(4) . . ?
C1 C2 Lu1 74.2(4) . . ?
C7 C2 Lu1 131.4(6) . . ?
C2 C3 C4 108.5(7) . . ?
C2 C3 C8 125.1(9) . . ?
C4 C3 C8 126.1(8) . . ?
C2 C3 Lu1 76.9(4) . . ?
C4 C3 Lu1 74.8(4) . . ?
C8 C3 Lu1 119.8(6) . . ?
C5 C4 C3 107.0(7) . . ?
C5 C4 C9 125.7(8) . . ?
C3 C4 C9 126.9(8) . . ?
C5 C4 Lu1 73.9(4) . . ?
C3 C4 Lu1 73.3(4) . . ?
C9 C4 Lu1 122.9(5) . . ?
C1 C5 C4 108.2(7) . . ?
C1 C5 C10 126.1(8) . . ?
C4 C5 C10 125.4(8) . . ?
C1 C5 Lu1 76.4(4) . . ?
C4 C5 Lu1 74.4(4) . . ?
C10 C5 Lu1 120.1(5) . . ?
C12 C11 C15 107.3(8) . . ?
C12 C11 C16 113.7(11) . . ?
C15 C11 C16 138.8(12) . . ?
C12 C11 C16A 138.4(11) . . ?
C15 C11 C16A 113.8(11) . . ?
C12 C11 Lu1 73.0(5) . . ?
C15 C11 Lu1 75.0(5) . . ?
C16 C11 Lu1 119.7(8) . . ?
C11 C12 C13 108.3(8) . . ?
C11 C12 C17A 116.1(12) . . ?
C13 C12 C17A 135.3(12) . . ?
C11 C12 C17 139.0(11) . . ?
C13 C12 C17 112.7(11) . . ?
C11 C12 Lu1 75.7(4) . . ?
C13 C12 Lu1 77.0(5) . . ?
C17 C12 Lu1 112.2(9) . . ?
C14 C13 C12 108.4(8) . . ?
C14 C13 C18A 123.0(11) . . ?
C12 C13 C18A 127.5(11) . . ?
C14 C13 C18 140.7(12) . . ?
C12 C13 C18 110.8(12) . . ?
C14 C13 Lu1 75.4(4) . . ?
C12 C13 Lu1 72.0(4) . . ?
C18 C13 Lu1 114.5(10) . . ?
C15 C14 C13 108.9(8) . . ?
C15 C14 C19 136.4(12) . . ?
C13 C14 C19 113.6(11) . . ?
C15 C14 C19A 115.5(10) . . ?
C13 C14 C19A 134.2(11) . . ?
C15 C14 Lu1 74.0(5) . . ?
C13 C14 Lu1 74.1(5) . . ?
C19 C14 Lu1 126.8(9) . . ?
C14 C15 C11 107.0(8) . . ?
C14 C15 C20A 137.3(15) . . ?
C11 C15 C20A 114.4(14) . . ?
C14 C15 C20 116.4(10) . . ?
C11 C15 C20 135.8(11) . . ?
C14 C15 Lu1 75.6(5) . . ?
C11 C15 Lu1 73.1(5) . . ?
C20 C15 Lu1 124.3(8) . . ?

_refine_diff_density_max         1.327
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.154

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef24
_database_code_depnum_ccdc_archive 'CCDC 1415195'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me5)2Gd]2(μ-η2:η2-N2)'
_chemical_name_common            1-Gd
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Gd2 N2'
_chemical_formula_weight         883.40

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.4239(19)
_cell_length_b                   14.4239(19)
_cell_length_c                   19.665(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4091.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9050
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.72

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_F_000             1768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.618
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.248
_exptl_absorpt_coefficient_mu    3.240
_shelx_estimated_absorpt_T_min   0.239
_shelx_estimated_absorpt_T_max   0.500
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2034
_exptl_absorpt_correction_T_max  0.5526
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48752
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.751
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5262
_reflns_number_gt                5068
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_max     0.946
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.248 x 0.296 x 0.618 mm was mounted on
a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The APEX2
program package was used to determine the unit-cell parameters and for data collection
(5 sec/frame scan time for a sphere of diffraction data).  The raw frame data was
processed using SAINT and SADABS to yield the reflection data file.  Subsequent
calculations were carried out using the SHELXTL program.  The diffraction symmetry
was 4/mmm and the systematic absences were consistent with the tetragonal space group
P-421c that was later determined to be correct. The structure was solved by direct methods
and refined on F2 by full-matrix least-squares techniques.  The analytical scattering
factors for neutral atoms were used throughout the analysis.  Hydrogen atoms were
included using a riding model.  The molecule was located about a two-fold rotation axis.
At convergence, wR2 = 0.0424 and Goof = 1.052 for 209 variables refined against 5262
data (0.73), R1 = 0.0169 for those 5068 data with I > 2.0sigma(I).  The absolute
structure was assigned by refinement of the Flack parameter. There were high residuals
present in the final difference-Fourier map.  It was not possible to determine the
nature of the residuals although it was probable that benzene or methylcyclohexane solvent
was present.  The SQUEEZE routine in the PLATON program package was used to account for
the electrons in the solvent accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+0.7242P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2196 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.023(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5262
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0169
_refine_ls_wR_factor_ref         0.0424
_refine_ls_wR_factor_gt          0.0418
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.84529(2) 0.53337(2) 0.84230(2) 0.01502(5) Uani 1 1 d . . . . .
N1 N 0.99121(16) 0.45806(17) 0.84667(14) 0.0199(5) Uani 1 1 d . . . . .
C1 C 0.7801(2) 0.3847(2) 0.90905(17) 0.0198(6) Uani 1 1 d . . . . .
C2 C 0.6999(2) 0.4368(2) 0.89288(16) 0.0212(6) Uani 1 1 d . . . . .
C3 C 0.7019(2) 0.5202(2) 0.93074(16) 0.0219(6) Uani 1 1 d . . . . .
C4 C 0.7842(2) 0.5200(2) 0.97061(16) 0.0231(6) Uani 1 1 d . . . . .
C5 C 0.8315(2) 0.4350(2) 0.95835(16) 0.0230(7) Uani 1 1 d . . . . .
C6 C 0.8048(3) 0.2905(2) 0.8821(2) 0.0333(8) Uani 1 1 d . . . . .
H6A H 0.8723 0.2857 0.8772 0.050 Uiso 1 1 calc R U . . .
H6B H 0.7754 0.2814 0.8376 0.050 Uiso 1 1 calc R U . . .
H6C H 0.7829 0.2428 0.9138 0.050 Uiso 1 1 calc R U . . .
C7 C 0.6215(2) 0.4031(3) 0.8493(2) 0.0321(8) Uani 1 1 d . . . . .
H7A H 0.5872 0.3547 0.8736 0.048 Uiso 1 1 calc R U . . .
H7B H 0.6463 0.3777 0.8068 0.048 Uiso 1 1 calc R U . . .
H7C H 0.5798 0.4549 0.8390 0.048 Uiso 1 1 calc R U . . .
C8 C 0.6230(3) 0.5868(3) 0.9391(2) 0.0354(9) Uani 1 1 d . . . . .
H8A H 0.5894 0.5923 0.8960 0.053 Uiso 1 1 calc R U . . .
H8B H 0.6471 0.6477 0.9524 0.053 Uiso 1 1 calc R U . . .
H8C H 0.5808 0.5639 0.9744 0.053 Uiso 1 1 calc R U . . .
C9 C 0.8120(3) 0.5952(3) 1.02013(19) 0.0381(9) Uani 1 1 d . . . . .
H9A H 0.7971 0.6560 1.0008 0.057 Uiso 1 1 calc R U . . .
H9B H 0.8789 0.5915 1.0288 0.057 Uiso 1 1 calc R U . . .
H9C H 0.7782 0.5869 1.0629 0.057 Uiso 1 1 calc R U . . .
C10 C 0.9162(3) 0.3989(3) 0.9949(2) 0.0333(8) Uani 1 1 d . . . . .
H10A H 0.8984 0.3472 1.0245 0.050 Uiso 1 1 calc R U . . .
H10B H 0.9432 0.4487 1.0225 0.050 Uiso 1 1 calc R U . . .
H10C H 0.9619 0.3775 0.9616 0.050 Uiso 1 1 calc R U . . .
C11 C 0.8092(3) 0.5853(2) 0.71178(18) 0.0291(8) Uani 1 1 d . . . . .
C12 C 0.7322(2) 0.6172(2) 0.74918(18) 0.0258(7) Uani 1 1 d . . . . .
C13 C 0.7623(3) 0.6885(2) 0.79297(19) 0.0290(7) Uani 1 1 d . . . . .
C14 C 0.8579(3) 0.6999(2) 0.7838(2) 0.0324(8) Uani 1 1 d . . . . .
C15 C 0.8875(2) 0.6377(3) 0.73275(19) 0.0324(9) Uani 1 1 d . . . . .
C16 C 0.8039(5) 0.5189(3) 0.6540(2) 0.0601(15) Uani 1 1 d . . . . .
H16A H 0.7582 0.4707 0.6644 0.090 Uiso 1 1 calc R U . . .
H16B H 0.8647 0.4903 0.6469 0.090 Uiso 1 1 calc R U . . .
H16C H 0.7852 0.5520 0.6127 0.090 Uiso 1 1 calc R U . . .
C17 C 0.6328(3) 0.5926(3) 0.7346(3) 0.0502(13) Uani 1 1 d . . . . .
H17A H 0.6104 0.6297 0.6962 0.075 Uiso 1 1 calc R U . . .
H17B H 0.5948 0.6056 0.7748 0.075 Uiso 1 1 calc R U . . .
H17C H 0.6285 0.5266 0.7232 0.075 Uiso 1 1 calc R U . . .
C18 C 0.7009(4) 0.7524(3) 0.8350(3) 0.0642(15) Uani 1 1 d . . . . .
H18A H 0.7241 0.7550 0.8817 0.096 Uiso 1 1 calc R U . . .
H18B H 0.6372 0.7286 0.8350 0.096 Uiso 1 1 calc R U . . .
H18C H 0.7017 0.8148 0.8152 0.096 Uiso 1 1 calc R U . . .
C19 C 0.9177(5) 0.7699(4) 0.8207(4) 0.078(2) Uani 1 1 d . . . . .
H19A H 0.9832 0.7554 0.8131 0.117 Uiso 1 1 calc R U . . .
H19B H 0.9042 0.7675 0.8695 0.117 Uiso 1 1 calc R U . . .
H19C H 0.9043 0.8322 0.8034 0.117 Uiso 1 1 calc R U . . .
C20 C 0.9837(3) 0.6353(5) 0.7034(3) 0.077(2) Uani 1 1 d . . . . .
H20A H 0.9890 0.6818 0.6673 0.116 Uiso 1 1 calc R U . . .
H20B H 0.9959 0.5736 0.6845 0.116 Uiso 1 1 calc R U . . .
H20C H 1.0289 0.6487 0.7393 0.116 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Gd1 Cnt1 2.409 . ?
Gd1 Cnt2 2.429 . ?
Gd1 N1 2.363(2) 2_765 ?
Gd1 N1 2.370(2) . ?
Gd1 C14 2.670(3) . ?
Gd1 C4 2.679(3) . ?
Gd1 C1 2.685(3) . ?
Gd1 C5 2.695(3) . ?
Gd1 C15 2.698(3) . ?
Gd1 C2 2.707(3) . ?
Gd1 C3 2.709(3) . ?
Gd1 C13 2.717(3) . ?
Gd1 C11 2.724(3) . ?
Gd1 C12 2.735(3) . ?
N1 N1 1.236(5) 2_765 ?
N1 Gd1 2.363(2) 2_765 ?
C1 C2 1.416(5) . ?
C1 C5 1.420(5) . ?
C1 C6 1.502(5) . ?
C2 C3 1.415(5) . ?
C2 C7 1.500(4) . ?
C3 C4 1.423(5) . ?
C3 C8 1.499(5) . ?
C4 C5 1.424(5) . ?
C4 C9 1.512(5) . ?
C5 C10 1.510(5) . ?
C11 C12 1.410(5) . ?
C11 C15 1.420(5) . ?
C11 C16 1.488(6) . ?
C12 C13 1.410(5) . ?
C12 C17 1.504(5) . ?
C13 C14 1.400(5) . ?
C13 C18 1.522(5) . ?
C14 C15 1.412(6) . ?
C14 C19 1.514(6) . ?
C15 C20 1.504(5) . ?

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
Cnt1 Gd1 N1 103.1 . . ?
Cnt1 Gd1 N1 120.6 . 2_765 ?
Cnt2 Gd1 N1 121.3 . . ?
Cnt2 Gd1 N1 101.6 . 2_765 ?
Cnt1 Gd1 Cnt2 135.4 . . ?
N1 Gd1 N1 30.28(11) 2_765 . ?
N1 Gd1 C14 84.31(10) 2_765 . ?
N1 Gd1 C14 111.58(11) . . ?
N1 Gd1 C4 107.31(10) 2_765 . ?
N1 Gd1 C4 102.99(10) . . ?
C14 Gd1 C4 119.53(12) . . ?
N1 Gd1 C1 111.93(9) 2_765 . ?
N1 Gd1 C1 85.82(9) . . ?
C14 Gd1 C1 162.44(11) . . ?
C4 Gd1 C1 50.72(10) . . ?
N1 Gd1 C5 94.03(10) 2_765 . ?
N1 Gd1 C5 78.07(10) . . ?
C14 Gd1 C5 147.55(12) . . ?
C4 Gd1 C5 30.73(10) . . ?
C1 Gd1 C5 30.61(10) . . ?
N1 Gd1 C15 76.98(10) 2_765 . ?
N1 Gd1 C15 94.84(10) . . ?
C14 Gd1 C15 30.51(12) . . ?
C4 Gd1 C15 150.04(11) . . ?
C1 Gd1 C15 156.24(12) . . ?
C5 Gd1 C15 170.68(11) . . ?
N1 Gd1 C2 141.88(9) 2_765 . ?
N1 Gd1 C2 116.03(9) . . ?
C14 Gd1 C2 132.37(11) . . ?
C4 Gd1 C2 50.38(10) . . ?
C1 Gd1 C2 30.45(10) . . ?
C5 Gd1 C2 50.26(10) . . ?
C15 Gd1 C2 139.05(10) . . ?
N1 Gd1 C3 137.92(10) 2_765 . ?
N1 Gd1 C3 128.50(9) . . ?
C14 Gd1 C3 113.06(12) . . ?
C4 Gd1 C3 30.62(10) . . ?
C1 Gd1 C3 50.41(9) . . ?
C5 Gd1 C3 50.44(10) . . ?
C15 Gd1 C3 136.39(10) . . ?
C2 Gd1 C3 30.29(10) . . ?
N1 Gd1 C13 114.17(10) 2_765 . ?
N1 Gd1 C13 141.41(10) . . ?
C14 Gd1 C13 30.10(11) . . ?
C4 Gd1 C13 104.52(11) . . ?
C1 Gd1 C13 132.72(11) . . ?
C5 Gd1 C13 134.72(11) . . ?
C15 Gd1 C13 49.81(11) . . ?
C2 Gd1 C13 102.34(10) . . ?
C3 Gd1 C13 87.17(11) . . ?
N1 Gd1 C11 102.16(10) 2_765 . ?
N1 Gd1 C11 109.27(10) . . ?
C14 Gd1 C11 50.15(11) . . ?
C4 Gd1 C11 147.59(11) . . ?
C1 Gd1 C11 127.85(11) . . ?
C5 Gd1 C11 158.24(11) . . ?
C15 Gd1 C11 30.36(11) . . ?
C2 Gd1 C11 109.86(11) . . ?
C3 Gd1 C11 118.57(10) . . ?
C13 Gd1 C11 49.67(11) . . ?
N1 Gd1 C12 126.64(10) 2_765 . ?
N1 Gd1 C12 139.19(10) . . ?
C14 Gd1 C12 49.76(11) . . ?
C4 Gd1 C12 117.79(11) . . ?
C1 Gd1 C12 118.15(10) . . ?
C5 Gd1 C12 139.11(10) . . ?
C15 Gd1 C12 49.69(10) . . ?
C2 Gd1 C12 90.65(10) . . ?
C3 Gd1 C12 90.31(10) . . ?
C13 Gd1 C12 29.99(11) . . ?
C11 Gd1 C12 29.93(11) . . ?
N1 N1 Gd1 75.2(2) 2_765 2_765 ?
N1 N1 Gd1 74.5(2) 2_765 . ?
Gd1 N1 Gd1 149.42(11) 2_765 . ?
C2 C1 C5 108.0(3) . . ?
C2 C1 C6 126.5(3) . . ?
C5 C1 C6 125.4(3) . . ?
C2 C1 Gd1 75.66(17) . . ?
C5 C1 Gd1 75.09(18) . . ?
C6 C1 Gd1 117.8(2) . . ?
C3 C2 C1 108.4(3) . . ?
C3 C2 C7 126.3(3) . . ?
C1 C2 C7 124.9(3) . . ?
C3 C2 Gd1 74.92(17) . . ?
C1 C2 Gd1 73.90(17) . . ?
C7 C2 Gd1 122.7(2) . . ?
C2 C3 C4 107.8(3) . . ?
C2 C3 C8 125.9(3) . . ?
C4 C3 C8 125.1(3) . . ?
C2 C3 Gd1 74.79(17) . . ?
C4 C3 Gd1 73.55(17) . . ?
C8 C3 Gd1 127.3(2) . . ?
C3 C4 C5 107.9(3) . . ?
C3 C4 C9 125.1(3) . . ?
C5 C4 C9 126.9(3) . . ?
C3 C4 Gd1 75.83(17) . . ?
C5 C4 Gd1 75.23(18) . . ?
C9 C4 Gd1 117.9(2) . . ?
C1 C5 C4 107.8(3) . . ?
C1 C5 C10 124.9(3) . . ?
C4 C5 C10 127.1(3) . . ?
C1 C5 Gd1 74.30(18) . . ?
C4 C5 Gd1 74.04(18) . . ?
C10 C5 Gd1 121.7(2) . . ?
C12 C11 C15 107.6(3) . . ?
C12 C11 C16 124.6(4) . . ?
C15 C11 C16 127.3(4) . . ?
C12 C11 Gd1 75.45(19) . . ?
C15 C11 Gd1 73.8(2) . . ?
C16 C11 Gd1 123.5(3) . . ?
C11 C12 C13 108.3(3) . . ?
C11 C12 C17 125.1(4) . . ?
C13 C12 C17 125.6(4) . . ?
C11 C12 Gd1 74.63(19) . . ?
C13 C12 Gd1 74.32(19) . . ?
C17 C12 Gd1 126.3(2) . . ?
C14 C13 C12 108.1(3) . . ?
C14 C13 C18 124.9(4) . . ?
C12 C13 C18 126.4(4) . . ?
C14 C13 Gd1 73.08(19) . . ?
C12 C13 Gd1 75.69(18) . . ?
C18 C13 Gd1 124.2(3) . . ?
C13 C14 C15 108.4(3) . . ?
C13 C14 C19 125.3(5) . . ?
C15 C14 C19 126.3(4) . . ?
C13 C14 Gd1 76.82(19) . . ?
C15 C14 Gd1 75.82(19) . . ?
C19 C14 Gd1 115.6(3) . . ?
C14 C15 C11 107.7(3) . . ?
C14 C15 C20 124.6(5) . . ?
C11 C15 C20 127.6(5) . . ?
C14 C15 Gd1 73.67(19) . . ?
C11 C15 Gd1 75.9(2) . . ?
C20 C15 Gd1 120.1(3) . . ?

_refine_diff_density_max         1.102
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.072



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef25
_database_code_depnum_ccdc_archive 'CCDC 1415196'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me5)2Tb]2(μ-η2:η2-N2)'
_chemical_name_common            1-Tb
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 N2 Tb2'
_chemical_formula_weight         886.74

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.4075(15)
_cell_length_b                   14.4075(15)
_cell_length_c                   19.627(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4074.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9720
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      29.01

_exptl_crystal_description       rod
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.095
_exptl_absorpt_coefficient_mu    3.469
_shelx_estimated_absorpt_T_min   0.461
_shelx_estimated_absorpt_T_max   0.734
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5543
_exptl_absorpt_correction_T_max  0.7771
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48977
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.753
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5254
_reflns_number_gt                5092
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_max     0.953
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A purple crystal of approximate dimensions 0.095 x 0.109 x 0.264 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The
APEX2 program package was used to determine the unit-cell parameters and for data
collection (20 sec/frame scan time for a sphere of diffraction data).  The raw frame
data was processed using SAINT and SADABS to yield the reflection data file.
Subsequent calculations were carried out using the SHELXTL program.  The
diffraction symmetry was 4/mmm and the systematic absences were consistent with the
tetragonal space group P-421c that was later determined to be correct. The structure was
solved by direct methods and refined on F2 by full-matrix least-squares techniques.
The analytical scattering factors for neutral atoms were used throughout the analysis.
Hydrogen atoms were included using a riding model.  The molecule was located about a
two-fold rotation axis. At convergence, wR2 = 0.0377 and Goof = 1.028 for 209 variables
refined against 5254 data (0.73), R1 = 0.0159 for those 5092 data with I > 2.0sigma(I).
The absolute structure was assigned by refinement of the Flack parameter. There were high
residuals present in the final difference-Fourier map.  It was not possible to determine
the nature of the residuals although it was probable that benzene or methylcyclohexane
solvent was present.  The SQUEEZE routine in the PLATON program package was used to
account for the electrons in the solvent accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²+0.3204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2227 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.018(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5254
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0377
_refine_ls_wR_factor_gt          0.0372
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.84653(2) 0.53396(2) 0.84334(2) 0.01600(4) Uani 1 1 d . . . . .
N1 N 0.99084(15) 0.45804(15) 0.84699(13) 0.0218(4) Uani 1 1 d . . . . .
C1 C 0.7813(2) 0.3848(2) 0.90825(16) 0.0218(6) Uani 1 1 d . . . . .
C2 C 0.7009(2) 0.4371(2) 0.89173(14) 0.0217(6) Uani 1 1 d . . . . .
C3 C 0.70249(19) 0.5200(2) 0.93032(14) 0.0221(6) Uani 1 1 d . . . . .
C4 C 0.7842(2) 0.5194(2) 0.97062(15) 0.0250(6) Uani 1 1 d . . . . .
C5 C 0.8318(2) 0.4348(2) 0.95792(15) 0.0233(6) Uani 1 1 d . . . . .
C6 C 0.8057(2) 0.2906(2) 0.8807(2) 0.0352(8) Uani 1 1 d . . . . .
H6A H 0.8728 0.2873 0.8727 0.053 Uiso 1 1 calc R U . . .
H6B H 0.7726 0.2802 0.8378 0.053 Uiso 1 1 calc R U . . .
H6C H 0.7877 0.2429 0.9138 0.053 Uiso 1 1 calc R U . . .
C7 C 0.6221(2) 0.4032(2) 0.84814(19) 0.0345(7) Uani 1 1 d . . . . .
H7A H 0.5886 0.3538 0.8722 0.052 Uiso 1 1 calc R U . . .
H7B H 0.6467 0.3789 0.8051 0.052 Uiso 1 1 calc R U . . .
H7C H 0.5796 0.4547 0.8387 0.052 Uiso 1 1 calc R U . . .
C8 C 0.6225(2) 0.5866(3) 0.93880(19) 0.0377(8) Uani 1 1 d . . . . .
H8A H 0.5898 0.5932 0.8953 0.057 Uiso 1 1 calc R U . . .
H8B H 0.6462 0.6472 0.9532 0.057 Uiso 1 1 calc R U . . .
H8C H 0.5797 0.5626 0.9734 0.057 Uiso 1 1 calc R U . . .
C9 C 0.8116(3) 0.5938(3) 1.02106(18) 0.0396(8) Uani 1 1 d . . . . .
H9A H 0.7913 0.6545 1.0041 0.059 Uiso 1 1 calc R U . . .
H9B H 0.8791 0.5939 1.0267 0.059 Uiso 1 1 calc R U . . .
H9C H 0.7820 0.5813 1.0651 0.059 Uiso 1 1 calc R U . . .
C10 C 0.9164(2) 0.3985(3) 0.99490(19) 0.0352(8) Uani 1 1 d . . . . .
H10A H 0.8998 0.3425 1.0205 0.053 Uiso 1 1 calc R U . . .
H10B H 0.9394 0.4460 1.0264 0.053 Uiso 1 1 calc R U . . .
H10C H 0.9650 0.3834 0.9617 0.053 Uiso 1 1 calc R U . . .
C11 C 0.8104(2) 0.5865(2) 0.71356(17) 0.0311(7) Uani 1 1 d . . . . .
C12 C 0.7335(2) 0.6176(2) 0.75093(17) 0.0271(7) Uani 1 1 d . . . . .
C13 C 0.7638(2) 0.6893(2) 0.79529(18) 0.0312(7) Uani 1 1 d . . . . .
C14 C 0.8596(2) 0.7003(2) 0.78575(19) 0.0335(8) Uani 1 1 d . . . . .
C15 C 0.8886(2) 0.6384(2) 0.73474(17) 0.0320(8) Uani 1 1 d . . . . .
C16 C 0.8048(5) 0.5201(3) 0.6551(2) 0.0651(14) Uani 1 1 d . . . . .
H16A H 0.7610 0.4703 0.6661 0.098 Uiso 1 1 calc R U . . .
H16B H 0.8663 0.4935 0.6465 0.098 Uiso 1 1 calc R U . . .
H16C H 0.7834 0.5531 0.6143 0.098 Uiso 1 1 calc R U . . .
C17 C 0.6338(3) 0.5938(3) 0.7360(2) 0.0539(12) Uani 1 1 d . . . . .
H17A H 0.6122 0.6303 0.6970 0.081 Uiso 1 1 calc R U . . .
H17B H 0.5955 0.6081 0.7759 0.081 Uiso 1 1 calc R U . . .
H17C H 0.6288 0.5275 0.7254 0.081 Uiso 1 1 calc R U . . .
C18 C 0.7028(4) 0.7530(3) 0.8378(3) 0.0705(15) Uani 1 1 d . . . . .
H18A H 0.7251 0.7535 0.8850 0.106 Uiso 1 1 calc R U . . .
H18B H 0.6387 0.7305 0.8366 0.106 Uiso 1 1 calc R U . . .
H18C H 0.7054 0.8161 0.8192 0.106 Uiso 1 1 calc R U . . .
C19 C 0.9190(4) 0.7704(3) 0.8233(3) 0.080(2) Uani 1 1 d . . . . .
H19A H 0.9845 0.7597 0.8125 0.120 Uiso 1 1 calc R U . . .
H19B H 0.9095 0.7636 0.8725 0.120 Uiso 1 1 calc R U . . .
H19C H 0.9014 0.8333 0.8093 0.120 Uiso 1 1 calc R U . . .
C20 C 0.9845(3) 0.6357(5) 0.7046(3) 0.080(2) Uani 1 1 d . . . . .
H20A H 0.9911 0.6856 0.6710 0.120 Uiso 1 1 calc R U . . .
H20B H 0.9945 0.5756 0.6823 0.120 Uiso 1 1 calc R U . . .
H20C H 1.0306 0.6440 0.7408 0.120 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Tb1 Cnt1 2.392 . ?
Tb1 Cnt2 2.412 . ?
Tb1 N1 2.347(2) 2_765 ?
Tb1 N1 2.350(2) . ?
Tb1 C14 2.656(3) . ?
Tb1 C4 2.663(3) . ?
Tb1 C1 2.669(3) . ?
Tb1 C5 2.673(3) . ?
Tb1 C15 2.679(3) . ?
Tb1 C2 2.693(3) . ?
Tb1 C3 2.695(3) . ?
Tb1 C13 2.705(3) . ?
Tb1 C11 2.708(3) . ?
Tb1 C12 2.718(3) . ?
N1 N1 1.238(4) 2_765 ?
N1 Tb1 2.347(2) 2_765 ?
C1 C5 1.414(4) . ?
C1 C2 1.420(4) . ?
C1 C6 1.502(4) . ?
C2 C3 1.414(4) . ?
C2 C7 1.503(4) . ?
C3 C4 1.418(4) . ?
C3 C8 1.508(4) . ?
C4 C5 1.421(5) . ?
C4 C9 1.512(4) . ?
C5 C10 1.512(4) . ?
C11 C12 1.402(5) . ?
C11 C15 1.415(5) . ?
C11 C16 1.496(6) . ?
C12 C13 1.420(5) . ?
C12 C17 1.506(5) . ?
C13 C14 1.402(5) . ?
C13 C18 1.520(5) . ?
C14 C15 1.404(5) . ?
C14 C19 1.516(5) . ?
C15 C20 1.504(5) . ?

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
Cnt1 Tb1 N1 103.2 . . ?
Cnt1 Tb1 N1 121.3 2_765 . ?
Cnt2 Tb1 N1 121.4 . . ?
Cnt2 Tb1 N1 101.5 2_765 . ?
Cnt1 Tb1 Cnt2 135.1 . . ?
N1 Tb1 N1 30.55(11) 2_765 . ?
N1 Tb1 C14 84.13(10) 2_765 . ?
N1 Tb1 C14 111.71(10) . . ?
N1 Tb1 C4 108.17(9) 2_765 . ?
N1 Tb1 C4 103.47(9) . . ?
C14 Tb1 C4 119.62(11) . . ?
N1 Tb1 C1 112.12(9) 2_765 . ?
N1 Tb1 C1 85.54(8) . . ?
C14 Tb1 C1 162.64(10) . . ?
C4 Tb1 C1 50.95(9) . . ?
N1 Tb1 C5 94.57(9) 2_765 . ?
N1 Tb1 C5 78.21(9) . . ?
C14 Tb1 C5 147.78(11) . . ?
C4 Tb1 C5 30.88(10) . . ?
C1 Tb1 C5 30.69(9) . . ?
N1 Tb1 C15 76.74(9) 2_765 . ?
N1 Tb1 C15 94.90(9) . . ?
C14 Tb1 C15 30.52(11) . . ?
C4 Tb1 C15 150.13(11) . . ?
C1 Tb1 C15 155.75(11) . . ?
C5 Tb1 C15 171.03(10) . . ?
N1 Tb1 C2 142.43(9) 2_765 . ?
N1 Tb1 C2 115.94(9) . . ?
C14 Tb1 C2 132.29(10) . . ?
C4 Tb1 C2 50.62(9) . . ?
C1 Tb1 C2 30.70(9) . . ?
C5 Tb1 C2 50.54(9) . . ?
C15 Tb1 C2 138.43(9) . . ?
N1 Tb1 C3 138.86(9) 2_765 . ?
N1 Tb1 C3 128.84(9) . . ?
C14 Tb1 C3 113.06(11) . . ?
C4 Tb1 C3 30.70(9) . . ?
C1 Tb1 C3 50.68(9) . . ?
C5 Tb1 C3 50.65(9) . . ?
C15 Tb1 C3 136.09(9) . . ?
C2 Tb1 C3 30.44(9) . . ?
N1 Tb1 C13 114.19(9) 2_765 . ?
N1 Tb1 C13 141.75(9) . . ?
C14 Tb1 C13 30.30(11) . . ?
C4 Tb1 C13 104.11(10) . . ?
C1 Tb1 C13 132.64(10) . . ?
C5 Tb1 C13 134.48(10) . . ?
C15 Tb1 C13 50.03(10) . . ?
C2 Tb1 C13 102.02(10) . . ?
C3 Tb1 C13 86.75(10) . . ?
N1 Tb1 C11 101.94(10) 2_765 . ?
N1 Tb1 C11 109.19(10) . . ?
C14 Tb1 C11 50.30(10) . . ?
C4 Tb1 C11 147.12(10) . . ?
C1 Tb1 C11 127.32(10) . . ?
C5 Tb1 C11 157.76(10) . . ?
C15 Tb1 C11 30.46(10) . . ?
C2 Tb1 C11 109.07(10) . . ?
C3 Tb1 C11 117.96(10) . . ?
C13 Tb1 C11 49.93(11) . . ?
N1 Tb1 C12 126.61(9) 2_765 . ?
N1 Tb1 C12 139.13(9) . . ?
C14 Tb1 C12 50.12(10) . . ?
C4 Tb1 C12 117.32(10) . . ?
C1 Tb1 C12 117.67(9) . . ?
C5 Tb1 C12 138.65(10) . . ?
C15 Tb1 C12 49.89(9) . . ?
C2 Tb1 C12 89.90(9) . . ?
C3 Tb1 C12 89.69(10) . . ?
C13 Tb1 C12 30.35(10) . . ?
C11 Tb1 C12 29.95(10) . . ?
N1 N1 Tb1 74.9(2) 2_765 2_765 ?
N1 N1 Tb1 74.6(2) 2_765 . ?
Tb1 N1 Tb1 149.24(11) 2_765 . ?
C5 C1 C2 107.9(3) . . ?
C5 C1 C6 126.0(3) . . ?
C2 C1 C6 126.1(3) . . ?
C5 C1 Tb1 74.81(16) . . ?
C2 C1 Tb1 75.59(16) . . ?
C6 C1 Tb1 118.2(2) . . ?
C3 C2 C1 108.2(3) . . ?
C3 C2 C7 126.3(3) . . ?
C1 C2 C7 125.0(3) . . ?
C3 C2 Tb1 74.84(16) . . ?
C1 C2 Tb1 73.71(16) . . ?
C7 C2 Tb1 123.8(2) . . ?
C2 C3 C4 107.9(3) . . ?
C2 C3 C8 125.7(3) . . ?
C4 C3 C8 125.2(3) . . ?
C2 C3 Tb1 74.72(15) . . ?
C4 C3 Tb1 73.41(16) . . ?
C8 C3 Tb1 127.6(2) . . ?
C3 C4 C5 108.0(3) . . ?
C3 C4 C9 125.2(3) . . ?
C5 C4 C9 126.7(3) . . ?
C3 C4 Tb1 75.90(16) . . ?
C5 C4 Tb1 74.95(16) . . ?
C9 C4 Tb1 118.1(2) . . ?
C1 C5 C4 108.0(3) . . ?
C1 C5 C10 124.7(3) . . ?
C4 C5 C10 127.0(3) . . ?
C1 C5 Tb1 74.50(16) . . ?
C4 C5 Tb1 74.17(17) . . ?
C10 C5 Tb1 121.7(2) . . ?
C12 C11 C15 107.8(3) . . ?
C12 C11 C16 124.3(4) . . ?
C15 C11 C16 127.3(4) . . ?
C12 C11 Tb1 75.45(18) . . ?
C15 C11 Tb1 73.64(18) . . ?
C16 C11 Tb1 123.6(2) . . ?
C11 C12 C13 108.1(3) . . ?
C11 C12 C17 125.4(4) . . ?
C13 C12 C17 125.3(3) . . ?
C11 C12 Tb1 74.60(17) . . ?
C13 C12 Tb1 74.29(17) . . ?
C17 C12 Tb1 126.9(2) . . ?
C14 C13 C12 107.6(3) . . ?
C14 C13 C18 125.0(4) . . ?
C12 C13 C18 126.7(4) . . ?
C14 C13 Tb1 72.92(18) . . ?
C12 C13 Tb1 75.36(17) . . ?
C18 C13 Tb1 124.3(3) . . ?
C13 C14 C15 108.4(3) . . ?
C13 C14 C19 124.5(4) . . ?
C15 C14 C19 127.0(4) . . ?
C13 C14 Tb1 76.77(18) . . ?
C15 C14 Tb1 75.64(17) . . ?
C19 C14 Tb1 115.8(3) . . ?
C14 C15 C11 108.0(3) . . ?
C14 C15 C20 124.8(4) . . ?
C11 C15 C20 127.0(4) . . ?
C14 C15 Tb1 73.85(18) . . ?
C11 C15 Tb1 75.91(18) . . ?
C20 C15 Tb1 120.4(2) . . ?

_refine_diff_density_max         1.057
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.063



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef35
_database_code_depnum_ccdc_archive 'CCDC 1415197'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me4H)2(THF)Gd]2(μ-η2:η2-N2)'
_chemical_name_common            2-Gd
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H84 Gd2 N2 O2'
_chemical_formula_weight         1155.77

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.2453(7)
_cell_length_b                   13.9938(6)
_cell_length_c                   25.6281(11)
_cell_angle_alpha                90
_cell_angle_beta                 104.7734(4)
_cell_angle_gamma                90
_cell_volume                     5286.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      29.02

_exptl_crystal_description       irregular
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             2360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.237
_exptl_absorpt_coefficient_mu    2.529
_shelx_estimated_absorpt_T_min   0.451
_shelx_estimated_absorpt_T_max   0.586
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5341
_exptl_absorpt_correction_T_max  0.6846
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32162
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.644
_diffrn_reflns_theta_max         29.209
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6785
_reflns_number_gt                6008
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.9-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A green crystal of approximate dimensions 0.237 x 0.280 x 0.374 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The APEX2
program package was used to determine the unit-cell parameters and for data collection
(10 sec/frame scan time for a sphere of diffraction data).  The raw frame data was
processed using SAINT and SADABS to yield the reflection data file.  Subsequent
calculations were carried out using the SHELXTL program.  The diffraction symmetry
was 2/m and the systematic absences were consistent with the monoclinic space groups
Cc and C2/c.  It was later determined that space group C2/c was correct.
The structure was solved by direct methods and refined on F2 by full-matrix least-squares
techniques.  The analytical scattering factors for neutral atoms were used throughout
the analysis.  Hydrogen atom H(28) was located from a difference-Fourier map and refined
(x,y,z and Uiso).  The remaining hydrogen atoms were included using a riding model.  The
molecule was located about a two-fold rotation axis.  A methyl carbon atom on one
tetramethylcyclopentadienyl ligand was disordered over two positions (C(16) / C(19))
and included using multiple components with partial site-occupancy factors.  The ring
hydrogen atom associated with the disordered tetramethylcyclopentadienyl ligand was not
included in the refinement.  There was a molecule of toluene solvent present (two per
dimeric formula-unit).  The solvent was disordered.  Carbon atoms C(24)-C(27) were
included as above. At convergence, wR2 = 0.0449 and Goof = 1.071 for 350 variables
refined against 6785 data (0.73), R1 = 0.0190 for those 6008 data with I > 2.0sigma(I).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0129P)²+9.7966P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6785
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0449
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.60734(2) 0.50451(2) 0.33167(2) 0.01700(3) Uani 1 1 d . . . . .
O1 O 0.74359(9) 0.48480(10) 0.29613(5) 0.0260(3) Uani 1 1 d . . . . .
N1 N 0.47012(11) 0.50110(10) 0.26268(6) 0.0202(3) Uani 1 1 d . . . . .
C1 C 0.53479(13) 0.67251(13) 0.35230(8) 0.0262(4) Uani 1 1 d . . . . .
C2 C 0.59306(14) 0.64785(13) 0.40254(8) 0.0258(4) Uani 1 1 d . . . . .
C3 C 0.68414(13) 0.65346(12) 0.39835(7) 0.0227(4) Uani 1 1 d . . . . .
C4 C 0.68183(13) 0.68337(12) 0.34509(7) 0.0218(4) Uani 1 1 d . . . . .
C5 C 0.58982(13) 0.69463(13) 0.31667(8) 0.0242(4) Uani 1 1 d . . . . .
H5A H 0.5684 0.7137 0.2801 0.029 Uiso 1 1 calc R U . . .
C6 C 0.43346(15) 0.68328(16) 0.33982(11) 0.0397(5) Uani 1 1 d . . . . .
H6A H 0.4098 0.6437 0.3647 0.060 Uiso 1 1 calc R U . . .
H6B H 0.4063 0.6628 0.3026 0.060 Uiso 1 1 calc R U . . .
H6C H 0.4182 0.7504 0.3440 0.060 Uiso 1 1 calc R U . . .
C7 C 0.5650(2) 0.63771(18) 0.45474(10) 0.0464(6) Uani 1 1 d . . . . .
H7A H 0.5092 0.5997 0.4484 0.070 Uiso 1 1 calc R U . . .
H7B H 0.5541 0.7012 0.4680 0.070 Uiso 1 1 calc R U . . .
H7C H 0.6133 0.6057 0.4816 0.070 Uiso 1 1 calc R U . . .
C8 C 0.76804(15) 0.64155(15) 0.44400(8) 0.0317(4) Uani 1 1 d . . . . .
H8A H 0.8197 0.6258 0.4294 0.048 Uiso 1 1 calc R U . . .
H8B H 0.7585 0.5899 0.4678 0.048 Uiso 1 1 calc R U . . .
H8C H 0.7805 0.7012 0.4646 0.048 Uiso 1 1 calc R U . . .
C9 C 0.76166(14) 0.70957(14) 0.32376(8) 0.0286(4) Uani 1 1 d . . . . .
H9A H 0.7492 0.6918 0.2856 0.043 Uiso 1 1 calc R U . . .
H9B H 0.8156 0.6754 0.3442 0.043 Uiso 1 1 calc R U . . .
H9C H 0.7723 0.7786 0.3275 0.043 Uiso 1 1 calc R U . . .
C10 C 0.53431(15) 0.38044(13) 0.38852(8) 0.0279(4) Uani 1 1 d . . . . .
C11 C 0.54808(15) 0.32599(13) 0.34446(8) 0.0269(4) Uani 1 1 d . . . . .
C12 C 0.64236(15) 0.31199(13) 0.35188(8) 0.0264(4) Uani 1 1 d . . . . .
C13 C 0.68774(15) 0.35704(13) 0.40077(8) 0.0283(4) Uani 1 1 d . . . . .
C14 C 0.62030(16) 0.39835(14) 0.42329(8) 0.0309(5) Uani 1 1 d . . . . .
C15 C 0.44359(17) 0.40567(16) 0.39820(9) 0.0374(5) Uani 1 1 d . . . . .
H15A H 0.4523 0.4513 0.4281 0.056 Uiso 1 1 calc R U . . .
H15B H 0.4146 0.3477 0.4073 0.056 Uiso 1 1 calc R U . . .
H15C H 0.4048 0.4344 0.3655 0.056 Uiso 1 1 calc R U . . .
C16 C 0.4796(2) 0.2798(3) 0.30647(14) 0.0253(8) Uani 0.555(5) 1 d . . P . .
H16A H 0.5065 0.2418 0.2824 0.038 Uiso 0.555(5) 1 calc R U P . .
H16B H 0.4383 0.3274 0.2853 0.038 Uiso 0.555(5) 1 calc R U P . .
H16C H 0.4459 0.2378 0.3249 0.038 Uiso 0.555(5) 1 calc R U P . .
C17 C 0.68603(15) 0.25215(15) 0.31636(9) 0.0328(5) Uani 1 1 d . . . . .
H17A H 0.6393 0.2147 0.2913 0.049 Uiso 1 1 calc R U . . .
H17B H 0.7305 0.2088 0.3389 0.049 Uiso 1 1 calc R U . . .
H17C H 0.7166 0.2941 0.2959 0.049 Uiso 1 1 calc R U . . .
C18 C 0.78619(17) 0.34678(17) 0.43045(9) 0.0389(5) Uani 1 1 d . . . . .
H18A H 0.8201 0.3202 0.4061 0.058 Uiso 1 1 calc R U . . .
H18B H 0.7916 0.3039 0.4613 0.058 Uiso 1 1 calc R U . . .
H18C H 0.8110 0.4096 0.4432 0.058 Uiso 1 1 calc R U . . .
C19 C 0.6282(3) 0.4242(3) 0.47890(16) 0.0245(10) Uani 0.445(5) 1 d . . P . .
H19A H 0.6781 0.4698 0.4908 0.037 Uiso 0.445(5) 1 calc R U P . .
H19B H 0.6406 0.3668 0.5015 0.037 Uiso 0.445(5) 1 calc R U P . .
H19C H 0.5714 0.4534 0.4821 0.037 Uiso 0.445(5) 1 calc R U P . .
C20 C 0.83619(15) 0.47379(18) 0.32860(9) 0.0356(5) Uani 1 1 d . . . . .
H20A H 0.8473 0.4073 0.3419 0.043 Uiso 1 1 calc R U . . .
H20B H 0.8483 0.5175 0.3600 0.043 Uiso 1 1 calc R U . . .
C21 C 0.89579(15) 0.49854(18) 0.29137(10) 0.0402(5) Uani 1 1 d . . . . .
H21A H 0.9556 0.4667 0.3028 0.048 Uiso 1 1 calc R U . . .
H21B H 0.9047 0.5684 0.2896 0.048 Uiso 1 1 calc R U . . .
C22 C 0.83982(15) 0.45931(19) 0.23771(9) 0.0398(5) Uani 1 1 d . . . . .
H22A H 0.8559 0.4911 0.2069 0.048 Uiso 1 1 calc R U . . .
H22B H 0.8483 0.3895 0.2352 0.048 Uiso 1 1 calc R U . . .
C23 C 0.74336(14) 0.48307(16) 0.23927(8) 0.0302(4) Uani 1 1 d . . . . .
H23A H 0.7250 0.5460 0.2224 0.036 Uiso 1 1 calc R U . . .
H23B H 0.7007 0.4340 0.2197 0.036 Uiso 1 1 calc R U . . .
C24 C 0.9384(3) 0.5311(4) 0.57699(19) 0.0313(12) Uani 0.580(9) 1 d . . P A 1
H24A H 0.9972 0.5524 0.5763 0.038 Uiso 0.580(9) 1 calc R U P A 1
C25 C 0.8789(11) 0.6005(10) 0.5875(6) 0.034(3) Uani 0.580(9) 1 d . . P A 1
H25A H 0.8975 0.6653 0.5925 0.041 Uiso 0.580(9) 1 calc R U P A 1
C26 C 0.7929(5) 0.5743(3) 0.59050(17) 0.0369(13) Uani 0.580(9) 1 d . . P A 1
H26A H 0.7525 0.6211 0.5978 0.044 Uiso 0.580(9) 1 calc R U P A 1
C27 C 0.7654(4) 0.4800(3) 0.5828(2) 0.0378(12) Uani 0.580(9) 1 d . . P A 1
H27A H 0.7056 0.4597 0.5819 0.045 Uiso 0.580(9) 1 calc R U P A 1
C24B C 0.9736(5) 0.5094(4) 0.5594(3) 0.0340(16) Uani 0.420(9) 1 d . . P A 2
H24B H 1.0255 0.5071 0.5453 0.041 Uiso 0.420(9) 1 calc R U P A 2
C25B C 0.9366(7) 0.5917(5) 0.5764(3) 0.046(2) Uani 0.420(9) 1 d . . P A 2
H25B H 0.9658 0.6515 0.5757 0.055 Uiso 0.420(9) 1 calc R U P A 2
C26B C 0.8589(16) 0.5874(12) 0.5940(8) 0.043(5) Uani 0.420(9) 1 d . . P A 2
H26B H 0.8348 0.6442 0.6052 0.051 Uiso 0.420(9) 1 calc R U P A 2
C27B C 0.8157(6) 0.5020(5) 0.5954(2) 0.0416(19) Uani 0.420(9) 1 d . . P A 2
H27B H 0.7658 0.5029 0.6113 0.050 Uiso 0.420(9) 1 calc R U P A 2
C28 C 0.8367(2) 0.41379(18) 0.57623(10) 0.0495(7) Uani 1 1 d . . . . .
C29 C 0.91947(18) 0.42934(17) 0.56692(10) 0.0462(7) Uani 1 1 d . . . . .
C30 C 0.97376(18) 0.3484(2) 0.55374(14) 0.0687(10) Uani 1 1 d . . . . .
H30A H 0.9344 0.2927 0.5430 0.103 Uiso 1 1 calc R U . . .
H30B H 1.0226 0.3324 0.5855 0.103 Uiso 1 1 calc R U . . .
H30C H 0.9999 0.3670 0.5240 0.103 Uiso 1 1 calc R U . . .
H28 H 0.812(2) 0.348(2) 0.5749(12) 0.068(9) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Gd1 Cnt1 2.448 . ?
Gd1 Cnt2 2.459 . ?
Gd1 N1 2.3703(16) . ?
Gd1 N1 2.4057(15) 2_655 ?
Gd1 O1 2.4870(13) . ?
Gd1 C10 2.6840(19) . ?
Gd1 C5 2.6917(18) . ?
Gd1 C11 2.7048(18) . ?
Gd1 C1 2.7070(18) . ?
Gd1 C4 2.7338(18) . ?
Gd1 C14 2.7428(19) . ?
Gd1 C2 2.7516(18) . ?
Gd1 C3 2.7596(18) . ?
Gd1 C12 2.7695(18) . ?
Gd1 C13 2.7910(18) . ?
O1 C20 1.453(2) . ?
O1 C23 1.456(2) . ?
N1 N1 1.247(3) 2_655 ?
N1 Gd1 2.4057(15) 2_655 ?
C1 C2 1.408(3) . ?
C1 C5 1.423(3) . ?
C1 C6 1.503(3) . ?
C2 C3 1.422(3) . ?
C2 C7 1.512(3) . ?
C3 C4 1.419(3) . ?
C3 C8 1.507(3) . ?
C4 C5 1.415(3) . ?
C4 C9 1.501(3) . ?
C10 C14 1.407(3) . ?
C10 C11 1.421(3) . ?
C10 C15 1.508(3) . ?
C11 C16 1.391(4) . ?
C11 C12 1.415(3) . ?
C12 C13 1.416(3) . ?
C12 C17 1.511(3) . ?
C13 C14 1.424(3) . ?
C13 C18 1.507(3) . ?
C14 C19 1.445(4) . ?
C20 C21 1.516(3) . ?
C21 C22 1.524(3) . ?
C22 C23 1.518(3) . ?
C24 C25 1.401(17) . ?
C24 C29 1.463(5) . ?
C25 C26 1.382(13) . ?
C26 C27 1.383(6) . ?
C27 C28 1.470(6) . ?
C24B C25B 1.399(10) . ?
C24B C29 1.433(6) . ?
C25B C26B 1.373(19) . ?
C26B C27B 1.369(17) . ?
C27B C28 1.396(7) . ?
C28 C29 1.360(4) . ?
C29 C30 1.491(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
Cnt1 Gd1 O1 103.9 . . ?
Cnt1 Gd1 N1 103.3 . . ?
Cnt1 Gd1 N1 108.7 . 2_655 ?
Cnt2 Gd1 O1 102.3 . . ?
Cnt2 Gd1 N1 104.6 . . ?
Cnt2 Gd1 N1 116.2 . 2_655 ?
Cnt1 Gd1 Cnt2 130.1 . . ?
N1 Gd1 N1 30.25(7) . 2_655 ?
N1 Gd1 O1 112.65(5) . . ?
N1 Gd1 O1 82.61(5) 2_655 . ?
N1 Gd1 C10 89.00(6) . . ?
N1 Gd1 C10 111.56(6) 2_655 . ?
O1 Gd1 C10 128.90(5) . . ?
N1 Gd1 C5 82.92(5) . . ?
N1 Gd1 C5 82.57(5) 2_655 . ?
O1 Gd1 C5 96.84(5) . . ?
C10 Gd1 C5 132.62(6) . . ?
N1 Gd1 C11 79.24(6) . . ?
N1 Gd1 C11 90.57(5) 2_655 . ?
O1 Gd1 C11 106.14(5) . . ?
C10 Gd1 C11 30.59(6) . . ?
C5 Gd1 C11 154.99(6) . . ?
N1 Gd1 C1 80.58(5) . . ?
N1 Gd1 C1 95.35(6) 2_655 . ?
O1 Gd1 C1 126.07(5) . . ?
C10 Gd1 C1 102.07(6) . . ?
C5 Gd1 C1 30.56(6) . . ?
C11 Gd1 C1 127.79(6) . . ?
N1 Gd1 C4 111.81(5) . . ?
N1 Gd1 C4 103.08(5) 2_655 . ?
O1 Gd1 C4 77.80(5) . . ?
C10 Gd1 C4 137.77(6) . . ?
C5 Gd1 C4 30.22(6) . . ?
C11 Gd1 C4 166.23(6) . . ?
C1 Gd1 C4 50.03(6) . . ?
N1 Gd1 C14 119.01(6) . . ?
N1 Gd1 C14 139.42(6) 2_655 . ?
O1 Gd1 C14 111.65(5) . . ?
C10 Gd1 C14 30.03(7) . . ?
C5 Gd1 C14 129.83(6) . . ?
C11 Gd1 C14 49.41(6) . . ?
C1 Gd1 C14 104.30(6) . . ?
C4 Gd1 C14 116.83(6) . . ?
N1 Gd1 C2 107.68(6) . . ?
N1 Gd1 C2 125.22(5) 2_655 . ?
O1 Gd1 C2 122.45(5) . . ?
C10 Gd1 C2 89.98(6) . . ?
C5 Gd1 C2 49.61(6) . . ?
C11 Gd1 C2 120.55(6) . . ?
C1 Gd1 C2 29.88(6) . . ?
C4 Gd1 C2 49.44(5) . . ?
C14 Gd1 C2 80.23(6) . . ?
N1 Gd1 C3 129.16(5) . . ?
N1 Gd1 C3 131.25(5) 2_655 . ?
O1 Gd1 C3 92.78(5) . . ?
C10 Gd1 C3 108.76(6) . . ?
C5 Gd1 C3 49.67(6) . . ?
C11 Gd1 C3 136.44(6) . . ?
C1 Gd1 C3 49.69(6) . . ?
C4 Gd1 C3 29.95(5) . . ?
C14 Gd1 C3 87.27(6) . . ?
C2 Gd1 C3 29.90(6) . . ?
N1 Gd1 C12 102.20(6) . . ?
N1 Gd1 C12 100.98(5) 2_655 . ?
O1 Gd1 C12 79.71(5) . . ?
C10 Gd1 C12 49.92(6) . . ?
C5 Gd1 C12 174.61(6) . . ?
C11 Gd1 C12 29.92(6) . . ?
C1 Gd1 C12 151.30(6) . . ?
C4 Gd1 C12 144.39(6) . . ?
C14 Gd1 C12 49.05(6) . . ?
C2 Gd1 C12 129.02(6) . . ?
C3 Gd1 C12 126.00(6) . . ?
N1 Gd1 C13 128.29(6) . . ?
N1 Gd1 C13 130.29(5) 2_655 . ?
O1 Gd1 C13 82.98(5) . . ?
C10 Gd1 C13 49.70(6) . . ?
C5 Gd1 C13 146.40(6) . . ?
C11 Gd1 C13 49.19(6) . . ?
C1 Gd1 C13 130.80(6) . . ?
C4 Gd1 C13 119.73(6) . . ?
C14 Gd1 C13 29.80(6) . . ?
C2 Gd1 C13 102.48(6) . . ?
C3 Gd1 C13 96.73(6) . . ?
C12 Gd1 C13 29.49(6) . . ?
C20 O1 C23 108.99(15) . . ?
C20 O1 Gd1 125.61(11) . . ?
C23 O1 Gd1 125.39(11) . . ?
N1 N1 Gd1 76.45(14) 2_655 . ?
N1 N1 Gd1 73.31(13) 2_655 2_655 ?
Gd1 N1 Gd1 149.66(7) . 2_655 ?
C2 C1 C5 107.60(17) . . ?
C2 C1 C6 126.4(2) . . ?
C5 C1 C6 125.7(2) . . ?
C2 C1 Gd1 76.81(10) . . ?
C5 C1 Gd1 74.13(10) . . ?
C6 C1 Gd1 119.63(13) . . ?
C1 C2 C3 108.54(17) . . ?
C1 C2 C7 125.2(2) . . ?
C3 C2 C7 125.1(2) . . ?
C1 C2 Gd1 73.30(10) . . ?
C3 C2 Gd1 75.36(10) . . ?
C7 C2 Gd1 127.13(13) . . ?
C4 C3 C2 107.68(17) . . ?
C4 C3 C8 125.97(18) . . ?
C2 C3 C8 125.97(17) . . ?
C4 C3 Gd1 74.02(10) . . ?
C2 C3 Gd1 74.74(10) . . ?
C8 C3 Gd1 122.65(12) . . ?
C5 C4 C3 107.82(17) . . ?
C5 C4 C9 125.08(17) . . ?
C3 C4 C9 126.77(18) . . ?
C5 C4 Gd1 73.24(10) . . ?
C3 C4 Gd1 76.03(10) . . ?
C9 C4 Gd1 121.81(12) . . ?
C4 C5 C1 108.36(17) . . ?
C4 C5 Gd1 76.54(10) . . ?
C1 C5 Gd1 75.32(10) . . ?
C14 C10 C11 107.22(18) . . ?
C14 C10 C15 126.84(18) . . ?
C11 C10 C15 125.7(2) . . ?
C14 C10 Gd1 77.30(11) . . ?
C11 C10 Gd1 75.51(10) . . ?
C15 C10 Gd1 117.56(13) . . ?
C16 C11 C12 125.8(2) . . ?
C16 C11 C10 124.6(2) . . ?
C12 C11 C10 108.56(18) . . ?
C16 C11 Gd1 123.92(19) . . ?
C12 C11 Gd1 77.57(11) . . ?
C10 C11 Gd1 73.90(11) . . ?
C11 C12 C13 107.93(17) . . ?
C11 C12 C17 125.77(19) . . ?
C13 C12 C17 126.10(19) . . ?
C11 C12 Gd1 72.50(10) . . ?
C13 C12 Gd1 76.10(10) . . ?
C17 C12 Gd1 121.34(13) . . ?
C12 C13 C14 107.41(19) . . ?
C12 C13 C18 127.12(18) . . ?
C14 C13 C18 124.30(18) . . ?
C12 C13 Gd1 74.41(11) . . ?
C14 C13 Gd1 73.22(11) . . ?
C18 C13 Gd1 127.63(14) . . ?
C10 C14 C13 108.88(18) . . ?
C10 C14 C19 120.0(2) . . ?
C13 C14 C19 127.9(2) . . ?
C10 C14 Gd1 72.67(10) . . ?
C13 C14 Gd1 76.98(11) . . ?
C19 C14 Gd1 132.7(2) . . ?
O1 C20 C21 105.43(17) . . ?
C20 C21 C22 101.42(19) . . ?
C23 C22 C21 102.75(17) . . ?
O1 C23 C22 105.95(16) . . ?
C25 C24 C29 126.9(6) . . ?
C26 C25 C24 119.8(10) . . ?
C25 C26 C27 120.1(8) . . ?
C26 C27 C28 114.3(4) . . ?
C25B C24B C29 108.1(6) . . ?
C26B C25B C24B 121.1(9) . . ?
C27B C26B C25B 120.6(14) . . ?
C26B C27B C28 127.4(10) . . ?
C29 C28 C27B 103.1(5) . . ?
C29 C28 C27 131.7(3) . . ?
C28 C29 C24B 137.7(4) . . ?
C28 C29 C24 105.9(3) . . ?
C28 C29 C30 120.8(2) . . ?
C24B C29 C30 101.0(4) . . ?
C24 C29 C30 133.1(3) . . ?

_refine_diff_density_max         0.752
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.068

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mef37
_database_code_depnum_ccdc_archive 'CCDC 1415198'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(C5Me4H)2(THF)Dy]2(μ-η2:η2-N2)'
_chemical_name_common            2-Dy
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H68 Dy2 N2 O2'
_chemical_formula_weight         982.00

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.7376(15)
_cell_length_b                   14.1959(14)
_cell_length_c                   18.9717(18)
_cell_angle_alpha                90
_cell_angle_beta                 101.2185(11)
_cell_angle_gamma                90
_cell_volume                     4157.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    4590
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.27

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             1976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.137
_exptl_absorpt_coefficient_mu    3.603
_shelx_estimated_absorpt_T_min   0.404
_shelx_estimated_absorpt_T_max   0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5785
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Bruker TWINABS 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4928
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.949
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4928
_reflns_number_gt                4482
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.9-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
A green crystal of approximate dimensions 0.137 x 0.176 x 0.307 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The
APEX2 program package and the CELL_NOW program were used to determine the
unit-cell parameters.  Data was collected using a 15 sec/frame scan time for a
sphere of diffraction data.  The raw frame data was processed using SAINT and TWINABS
to yield the reflection data file (HKLF 5 format).  Subsequent calculations were
carried out using the SHELXTL program.  The diffraction symmetry was 2/m and the
systematic absences were consistent with the monoclinic space groups Cc and C2/c.
It was later determined that space group C2/c was correct. The structure was solved
by direct methods and refined on F2 by full-matrix least-squares techniques.  The
analytical scattering factors for neutral atoms were used throughout the analysis.
Hydrogen atoms were included using a riding model.  The molecule was located about
a two-fold rotation axis. At convergence, wR2 = 0.0790 and Goof = 1.078 for 235
variables refined against 4928 data (0.75), R1 = 0.0316 for those 4482 with
I > 2.0sigma(I).  The structure was refined as a two-component twin, BASF5 = 0.1165. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4928
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.04242(2) 0.76058(2) 0.14252(2) 0.01881(7) Uani 1 1 d . . . . .
O1 O 0.19926(18) 0.7851(2) 0.19118(15) 0.0264(6) Uani 1 1 d . . . . .
N1 N -0.0382(2) 0.7654(2) 0.23357(18) 0.0210(7) Uani 1 1 d . . . . .
C1 C -0.0721(3) 0.8739(3) 0.0629(2) 0.0244(9) Uani 1 1 d . . . . .
C2 C -0.0290(3) 0.9346(3) 0.1181(2) 0.0244(9) Uani 1 1 d . . . . .
C3 C 0.0574(3) 0.9482(3) 0.1081(2) 0.0251(9) Uani 1 1 d . . . . .
C4 C 0.0681(3) 0.8957(3) 0.0466(2) 0.0269(9) Uani 1 1 d . . . . .
C5 C -0.0116(3) 0.8510(3) 0.0192(2) 0.0288(9) Uani 1 1 d . . . . .
H5A H -0.0229 0.8117 -0.0221 0.035 Uiso 1 1 calc R U . . .
C6 C -0.1657(3) 0.8468(3) 0.0505(2) 0.0318(10) Uani 1 1 d . . . . .
H6A H -0.2003 0.9013 0.0598 0.048 Uiso 1 1 calc R U . . .
H6B H -0.1736 0.7953 0.0831 0.048 Uiso 1 1 calc R U . . .
H6C H -0.1847 0.8262 0.0007 0.048 Uiso 1 1 calc R U . . .
C7 C -0.0728(3) 0.9828(3) 0.1718(2) 0.0292(9) Uani 1 1 d . . . . .
H7A H -0.1339 0.9935 0.1505 0.044 Uiso 1 1 calc R U . . .
H7B H -0.0444 1.0433 0.1855 0.044 Uiso 1 1 calc R U . . .
H7C H -0.0686 0.9430 0.2146 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1227(3) 1.0154(3) 0.1489(2) 0.0344(10) Uani 1 1 d . . . . .
H8A H 0.0942 1.0571 0.1783 0.052 Uiso 1 1 calc R U . . .
H8B H 0.1480 1.0532 0.1150 0.052 Uiso 1 1 calc R U . . .
H8C H 0.1686 0.9798 0.1801 0.052 Uiso 1 1 calc R U . . .
C9 C 0.1433(3) 0.9011(3) 0.0077(3) 0.0368(11) Uani 1 1 d . . . . .
H9A H 0.1876 0.9437 0.0336 0.055 Uiso 1 1 calc R U . . .
H9B H 0.1228 0.9249 -0.0411 0.055 Uiso 1 1 calc R U . . .
H9C H 0.1682 0.8381 0.0054 0.055 Uiso 1 1 calc R U . . .
C10 C 0.1069(3) 0.5888(3) 0.1240(2) 0.0251(9) Uani 1 1 d . . . . .
C11 C 0.0681(3) 0.6186(3) 0.0538(2) 0.0256(9) Uani 1 1 d . . . . .
C12 C -0.0225(3) 0.6202(3) 0.0490(2) 0.0248(9) Uani 1 1 d . . . . .
C13 C -0.0408(3) 0.5948(3) 0.1164(2) 0.0251(9) Uani 1 1 d . . . . .
C14 C 0.0400(3) 0.5753(3) 0.1630(2) 0.0251(9) Uani 1 1 d . . . . .
H14A H 0.0476 0.5564 0.2119 0.030 Uiso 1 1 calc R U . . .
C15 C 0.2007(3) 0.5638(3) 0.1505(3) 0.0335(10) Uani 1 1 d . . . . .
H15A H 0.2369 0.6005 0.1239 0.050 Uiso 1 1 calc R U . . .
H15B H 0.2091 0.4964 0.1428 0.050 Uiso 1 1 calc R U . . .
H15C H 0.2171 0.5782 0.2018 0.050 Uiso 1 1 calc R U . . .
C16 C 0.1127(3) 0.6313(3) -0.0089(2) 0.0353(10) Uani 1 1 d . . . . .
H16A H 0.0900 0.6877 -0.0360 0.053 Uiso 1 1 calc R U . . .
H16B H 0.1021 0.5760 -0.0403 0.053 Uiso 1 1 calc R U . . .
H16C H 0.1752 0.6386 0.0088 0.053 Uiso 1 1 calc R U . . .
C17 C -0.0882(3) 0.6299(3) -0.0200(2) 0.0334(10) Uani 1 1 d . . . . .
H17A H -0.0633 0.6669 -0.0546 0.050 Uiso 1 1 calc R U . . .
H17B H -0.1399 0.6619 -0.0103 0.050 Uiso 1 1 calc R U . . .
H17C H -0.1042 0.5673 -0.0399 0.050 Uiso 1 1 calc R U . . .
C18 C -0.1295(3) 0.5826(3) 0.1346(3) 0.0332(10) Uani 1 1 d . . . . .
H18A H -0.1309 0.6136 0.1805 0.050 Uiso 1 1 calc R U . . .
H18B H -0.1419 0.5154 0.1383 0.050 Uiso 1 1 calc R U . . .
H18C H -0.1733 0.6110 0.0967 0.050 Uiso 1 1 calc R U . . .
C19 C 0.2369(3) 0.7893(4) 0.2671(2) 0.0391(11) Uani 1 1 d . . . . .
H19A H 0.2269 0.7293 0.2908 0.047 Uiso 1 1 calc R U . . .
H19B H 0.2103 0.8410 0.2903 0.047 Uiso 1 1 calc R U . . .
C20 C 0.3323(4) 0.8063(4) 0.2737(3) 0.0484(13) Uani 1 1 d . . . . .
H20A H 0.3661 0.7696 0.3140 0.058 Uiso 1 1 calc R U . . .
H20B H 0.3463 0.8740 0.2815 0.058 Uiso 1 1 calc R U . . .
C21 C 0.3508(3) 0.7732(4) 0.2023(3) 0.0399(11) Uani 1 1 d . . . . .
H21A H 0.4013 0.8064 0.1900 0.048 Uiso 1 1 calc R U . . .
H21B H 0.3613 0.7044 0.2024 0.048 Uiso 1 1 calc R U . . .
C22 C 0.2680(3) 0.7991(3) 0.1510(2) 0.0322(10) Uani 1 1 d . . . . .
H22A H 0.2698 0.8655 0.1355 0.039 Uiso 1 1 calc R U . . .
H22B H 0.2592 0.7581 0.1080 0.039 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Dy1 Cnt1 2.421 . ?
Dy1 Cnt2 2.412 . ?
Dy1 N1 2.335(3) . ?
Dy1 N1 2.366(3) 2 ?
Dy1 O1 2.486(3) . ?
Dy1 C1 2.657(4) . ?
Dy1 C5 2.659(4) . ?
Dy1 C14 2.660(4) . ?
Dy1 C10 2.690(4) . ?
Dy1 C13 2.692(4) . ?
Dy1 C11 2.706(4) . ?
Dy1 C2 2.716(4) . ?
Dy1 C4 2.728(4) . ?
Dy1 C12 2.730(4) . ?
Dy1 C3 2.763(4) . ?
O1 C19 1.448(5) . ?
O1 C22 1.454(5) . ?
N1 N1 1.243(7) 2 ?
N1 Dy1 2.366(3) 2 ?
C1 C5 1.417(6) . ?
C1 C2 1.422(6) . ?
C1 C6 1.496(6) . ?
C2 C3 1.422(6) . ?
C2 C7 1.502(5) . ?
C3 C4 1.422(6) . ?
C3 C8 1.503(6) . ?
C4 C5 1.412(6) . ?
C4 C9 1.514(6) . ?
C10 C14 1.412(6) . ?
C10 C11 1.418(6) . ?
C10 C15 1.506(6) . ?
C11 C12 1.411(6) . ?
C11 C16 1.505(6) . ?
C12 C13 1.410(6) . ?
C12 C17 1.509(6) . ?
C13 C14 1.429(6) . ?
C13 C18 1.512(6) . ?
C19 C20 1.502(7) . ?
C20 C21 1.516(7) . ?
C21 C22 1.511(6) . ?

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
Cnt1 Dy1 O1 102.9 . . ?
Cnt1 Dy1 N1 105.8 . . ?
Cnt1 Dy1 N1 118.7 . 2 ?
Cnt2 Dy1 O1 105.2 . . ?
Cnt2 Dy1 N1 104.4 . . ?
Cnt2 Dy1 N1 109.5 . 2 ?
Cnt1 Dy1 Cnt2 127.0 . . ?
N1 Dy1 N1 30.66(16) . 2 ?
N1 Dy1 O1 111.38(11) . . ?
N1 Dy1 O1 81.05(11) 2 . ?
N1 Dy1 C1 89.81(12) . . ?
N1 Dy1 C1 113.62(12) 2 . ?
O1 Dy1 C1 129.89(11) . . ?
N1 Dy1 C5 120.68(13) . . ?
N1 Dy1 C5 142.64(12) 2 . ?
O1 Dy1 C5 112.56(12) . . ?
C1 Dy1 C5 30.93(13) . . ?
N1 Dy1 C14 84.00(11) . . ?
N1 Dy1 C14 83.06(11) 2 . ?
O1 Dy1 C14 97.19(12) . . ?
C1 Dy1 C14 130.88(13) . . ?
C5 Dy1 C14 126.48(13) . . ?
N1 Dy1 C10 113.33(12) . . ?
N1 Dy1 C10 103.87(12) 2 . ?
O1 Dy1 C10 78.62(11) . . ?
C1 Dy1 C10 134.92(13) . . ?
C5 Dy1 C10 112.75(13) . . ?
C14 Dy1 C10 30.60(12) . . ?
N1 Dy1 C13 81.18(11) . . ?
N1 Dy1 C13 95.83(12) 2 . ?
O1 Dy1 C13 127.10(11) . . ?
C1 Dy1 C13 99.93(13) . . ?
C5 Dy1 C13 101.47(13) . . ?
C14 Dy1 C13 30.97(12) . . ?
C10 Dy1 C13 50.67(13) . . ?
N1 Dy1 C11 130.55(12) . . ?
N1 Dy1 C11 132.53(12) 2 . ?
O1 Dy1 C11 94.46(12) . . ?
C1 Dy1 C11 105.31(13) . . ?
C5 Dy1 C11 82.69(13) . . ?
C14 Dy1 C11 50.40(12) . . ?
C10 Dy1 C11 30.47(12) . . ?
C13 Dy1 C11 50.25(13) . . ?
N1 Dy1 C2 80.42(11) . . ?
N1 Dy1 C2 93.04(11) 2 . ?
O1 Dy1 C2 106.50(11) . . ?
C1 Dy1 C2 30.68(12) . . ?
C5 Dy1 C2 50.22(13) . . ?
C14 Dy1 C2 155.12(13) . . ?
C10 Dy1 C2 162.96(13) . . ?
C13 Dy1 C2 126.39(13) . . ?
C11 Dy1 C2 132.69(13) . . ?
N1 Dy1 C4 130.21(12) . . ?
N1 Dy1 C4 132.78(12) 2 . ?
O1 Dy1 C4 83.34(12) . . ?
C1 Dy1 C4 50.74(13) . . ?
C5 Dy1 C4 30.35(13) . . ?
C14 Dy1 C4 143.22(13) . . ?
C10 Dy1 C4 116.21(13) . . ?
C13 Dy1 C4 128.44(13) . . ?
C11 Dy1 C4 92.82(14) . . ?
C2 Dy1 C4 49.96(13) . . ?
N1 Dy1 C12 108.25(12) . . ?
N1 Dy1 C12 125.96(12) 2 . ?
O1 Dy1 C12 124.22(11) . . ?
C1 Dy1 C12 86.90(13) . . ?
C5 Dy1 C12 76.43(13) . . ?
C14 Dy1 C12 50.15(12) . . ?
C10 Dy1 C12 49.97(12) . . ?
C13 Dy1 C12 30.14(12) . . ?
C11 Dy1 C12 30.08(13) . . ?
C2 Dy1 C12 117.57(12) . . ?
C4 Dy1 C12 99.51(13) . . ?
N1 Dy1 C3 103.33(11) . . ?
N1 Dy1 C3 103.14(12) 2 . ?
O1 Dy1 C3 80.14(11) . . ?
C1 Dy1 C3 50.34(13) . . ?
C5 Dy1 C3 49.78(13) . . ?
C14 Dy1 C3 172.67(12) . . ?
C10 Dy1 C3 142.28(13) . . ?
C13 Dy1 C3 149.30(13) . . ?
C11 Dy1 C3 122.75(12) . . ?
C2 Dy1 C3 30.06(12) . . ?
C4 Dy1 C3 30.01(12) . . ?
C12 Dy1 C3 126.04(12) . . ?
C19 O1 C22 108.3(3) . . ?
C19 O1 Dy1 124.0(3) . . ?
C22 O1 Dy1 127.7(2) . . ?
N1 N1 Dy1 76.0(3) 2 . ?
N1 N1 Dy1 73.3(3) 2 2 ?
Dy1 N1 Dy1 149.15(16) . 2 ?
C5 C1 C2 106.9(4) . . ?
C5 C1 C6 127.1(4) . . ?
C2 C1 C6 125.8(4) . . ?
C5 C1 Dy1 74.6(2) . . ?
C2 C1 Dy1 77.0(2) . . ?
C6 C1 Dy1 118.2(3) . . ?
C3 C2 C1 108.4(4) . . ?
C3 C2 C7 127.3(4) . . ?
C1 C2 C7 124.0(4) . . ?
C3 C2 Dy1 76.8(2) . . ?
C1 C2 Dy1 72.4(2) . . ?
C7 C2 Dy1 121.9(3) . . ?
C2 C3 C4 107.9(4) . . ?
C2 C3 C8 126.4(4) . . ?
C4 C3 C8 125.3(4) . . ?
C2 C3 Dy1 73.1(2) . . ?
C4 C3 Dy1 73.6(2) . . ?
C8 C3 Dy1 124.9(3) . . ?
C5 C4 C3 107.4(4) . . ?
C5 C4 C9 124.4(4) . . ?
C3 C4 C9 127.0(4) . . ?
C5 C4 Dy1 72.2(2) . . ?
C3 C4 Dy1 76.4(2) . . ?
C9 C4 Dy1 126.3(3) . . ?
C4 C5 C1 109.3(4) . . ?
C4 C5 Dy1 77.5(2) . . ?
C1 C5 Dy1 74.4(2) . . ?
C14 C10 C11 107.7(4) . . ?
C14 C10 C15 125.1(4) . . ?
C11 C10 C15 126.8(4) . . ?
C14 C10 Dy1 73.5(2) . . ?
C11 C10 Dy1 75.4(2) . . ?
C15 C10 Dy1 122.7(3) . . ?
C12 C11 C10 108.1(4) . . ?
C12 C11 C16 124.7(4) . . ?
C10 C11 C16 126.5(4) . . ?
C12 C11 Dy1 75.9(2) . . ?
C10 C11 Dy1 74.2(2) . . ?
C16 C11 Dy1 123.5(3) . . ?
C13 C12 C11 108.7(4) . . ?
C13 C12 C17 125.6(4) . . ?
C11 C12 C17 124.8(4) . . ?
C13 C12 Dy1 73.4(2) . . ?
C11 C12 Dy1 74.0(2) . . ?
C17 C12 Dy1 127.2(3) . . ?
C12 C13 C14 107.2(4) . . ?
C12 C13 C18 126.7(4) . . ?
C14 C13 C18 125.9(4) . . ?
C12 C13 Dy1 76.4(2) . . ?
C14 C13 Dy1 73.3(2) . . ?
C18 C13 Dy1 119.7(3) . . ?
C10 C14 C13 108.3(4) . . ?
C10 C14 Dy1 75.9(2) . . ?
C13 C14 Dy1 75.7(2) . . ?
O1 C19 C20 107.4(4) . . ?
C19 C20 C21 103.7(4) . . ?
C22 C21 C20 102.0(4) . . ?
O1 C22 C21 105.4(4) . . ?

_refine_diff_density_max         1.863
_refine_diff_density_min         -1.891
_refine_diff_density_rms         0.127

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dhw9
_database_code_depnum_ccdc_archive 'CCDC 1415199'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[(C5H4Me)2Y]2(μ-η2:η2-N2)'
_chemical_name_common            3-Y
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 N2 O2 Y2'
_chemical_formula_weight         666.51

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.9100(9)
_cell_length_b                   10.0376(7)
_cell_length_c                   12.6988(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.7802(9)
_cell_angle_gamma                90
_cell_volume                     1510.39(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      28.97

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.148
_exptl_absorpt_coefficient_mu    3.853
_shelx_estimated_absorpt_T_min   0.419
_shelx_estimated_absorpt_T_max   0.599
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4721
_exptl_absorpt_correction_T_max  0.6280
_exptl_absorpt_process_details   'Bruker SADABS 2014/2'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18124
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.235
_diffrn_reflns_theta_max         28.982
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3825
_reflns_number_gt                3517
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0208P)²+0.7780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3825
_refine_ls_number_parameters     260
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0193
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0443
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.17838(2) 0.93194(2) 0.50148(2) 0.00868(4) Uani 1 1 d . . . . .
O1 O 0.26935(8) 1.14524(9) 0.49524(8) 0.01416(19) Uani 1 1 d . . . . .
N1 N -0.01518(9) 0.94041(11) 0.49754(9) 0.0107(2) Uani 1 1 d . . . . .
C1 C 0.11632(13) 0.86304(15) 0.30048(11) 0.0175(3) Uani 1 1 d . . . . .
C2 C 0.21225(14) 0.94418(15) 0.29725(11) 0.0189(3) Uani 1 1 d . . . . .
C3 C 0.30574(12) 0.87405(15) 0.34721(11) 0.0172(3) Uani 1 1 d . . . . .
C4 C 0.26660(12) 0.74935(14) 0.38045(11) 0.0144(3) Uani 1 1 d . . . . .
C5 C 0.14889(12) 0.74186(14) 0.35230(11) 0.0147(3) Uani 1 1 d . . . . .
C6 C 0.07230(13) 0.62656(16) 0.36975(13) 0.0211(3) Uani 1 1 d . . . . .
C7 C 0.18417(12) 0.94256(14) 0.71256(11) 0.0141(3) Uani 1 1 d . . . . .
C8 C 0.29856(12) 0.94546(15) 0.69169(11) 0.0166(3) Uani 1 1 d . . . . .
C9 C 0.32435(12) 0.82162(15) 0.64828(11) 0.0170(3) Uani 1 1 d . . . . .
C10 C 0.22572(12) 0.74196(14) 0.64310(11) 0.0152(3) Uani 1 1 d . . . . .
C11 C 0.13914(11) 0.81614(13) 0.68378(10) 0.0130(3) Uani 1 1 d . . . . .
C12 C 0.02301(13) 0.76529(17) 0.69834(13) 0.0206(3) Uani 1 1 d . . . . .
C13 C 0.22528(12) 1.26486(14) 0.54224(12) 0.0158(3) Uani 1 1 d . . . . .
C14 C 0.28898(13) 1.37808(15) 0.49687(12) 0.0190(3) Uani 1 1 d . . . . .
C15 C 0.40593(13) 1.31812(15) 0.49173(12) 0.0201(3) Uani 1 1 d . . . . .
C16 C 0.37828(13) 1.17530(15) 0.45817(14) 0.0205(3) Uani 1 1 d . . . . .
H1A H 0.0395(15) 0.8840(18) 0.2723(14) 0.023(4) Uiso 1 1 d . . . . .
H2A H 0.2125(15) 1.031(2) 0.2710(15) 0.026(5) Uiso 1 1 d . . . . .
H3A H 0.3829(16) 0.9014(18) 0.3562(14) 0.025(5) Uiso 1 1 d . . . . .
H4A H 0.3089(14) 0.6827(18) 0.4145(14) 0.019(4) Uiso 1 1 d . . . . .
H6A H -0.0041(18) 0.652(2) 0.3522(16) 0.034(5) Uiso 1 1 d . . . . .
H6B H 0.0802(18) 0.596(2) 0.4426(18) 0.037(6) Uiso 1 1 d . . . . .
H6C H 0.0863(18) 0.553(2) 0.3284(18) 0.043(6) Uiso 1 1 d . . . . .
H7A H 0.1458(15) 1.0136(18) 0.7431(14) 0.021(4) Uiso 1 1 d . . . . .
H8A H 0.3478(16) 1.0196(19) 0.7041(14) 0.025(5) Uiso 1 1 d . . . . .
H9A H 0.3957(17) 0.795(2) 0.6303(15) 0.034(5) Uiso 1 1 d . . . . .
H10A H 0.2190(15) 0.6534(19) 0.6168(14) 0.025(5) Uiso 1 1 d . . . . .
H12A H -0.0309(18) 0.828(2) 0.6893(16) 0.038(6) Uiso 1 1 d . . . . .
H12B H 0.0200(17) 0.726(2) 0.7664(17) 0.038(6) Uiso 1 1 d . . . . .
H12C H -0.0022(18) 0.697(2) 0.6468(18) 0.042(6) Uiso 1 1 d . . . . .
H13A H 0.2385(14) 1.2613(16) 0.6174(14) 0.015(4) Uiso 1 1 d . . . . .
H13B H 0.1462(15) 1.2679(17) 0.5237(13) 0.018(4) Uiso 1 1 d . . . . .
H14A H 0.2890(16) 1.4518(19) 0.5385(16) 0.026(5) Uiso 1 1 d . . . . .
H14B H 0.2558(15) 1.3995(17) 0.4279(15) 0.021(4) Uiso 1 1 d . . . . .
H15A H 0.4488(16) 1.365(2) 0.4421(15) 0.031(5) Uiso 1 1 d . . . . .
H15B H 0.4499(16) 1.3181(18) 0.5624(15) 0.027(5) Uiso 1 1 d . . . . .
H16A H 0.3688(14) 1.1636(16) 0.3826(14) 0.015(4) Uiso 1 1 d . . . . .
H16B H 0.4342(17) 1.109(2) 0.4858(15) 0.032(5) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Y1 Cnt1 2.387 . ?
Y1 Cnt2 2.381 . ?
Y1 N1 2.3023(11) . ?
Y1 N1 2.3292(11) 3_576 ?
Y1 O1 2.4046(10) . ?
Y1 C10 2.6427(13) . ?
Y1 C9 2.6591(14) . ?
Y1 C3 2.6599(13) . ?
Y1 C2 2.6673(14) . ?
Y1 C11 2.6732(13) . ?
Y1 C4 2.6741(13) . ?
Y1 C1 2.6758(14) . ?
Y1 C7 2.6765(14) . ?
Y1 C8 2.6842(14) . ?
O1 C16 1.4556(17) . ?
O1 C13 1.4617(16) . ?
N1 N1 1.250(2) 3_576 ?
N1 Y1 2.3292(11) 3_576 ?
C1 C2 1.407(2) . ?
C1 C5 1.418(2) . ?
C2 C3 1.413(2) . ?
C3 C4 1.415(2) . ?
C4 C5 1.4135(19) . ?
C5 C6 1.504(2) . ?
C7 C11 1.4114(19) . ?
C7 C8 1.414(2) . ?
C8 C9 1.406(2) . ?
C9 C10 1.417(2) . ?
C10 C11 1.4114(19) . ?
C11 C12 1.5031(19) . ?
C13 C14 1.512(2) . ?
C14 C15 1.525(2) . ?
C15 C16 1.522(2) . ?

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
Cnt1 Y1 N1 104.0 . . ?
Cnt1 Y1 N1' 115.8 . . ?
Cnt1 Y1 O1 103.0 . . ?
Cnt1 Y1 N1 102.6 . . ?
Cnt1 Y1 N1' 109.4 . . ?
Cnt1 Y1 O1 103.9 . . ?
Cnt1 Y1 Cnt2 129.1 . . ?
N1 Y1 N1 31.30(5) . 3_576 ?
N1 Y1 O1 114.83(4) . . ?
N1 Y1 O1 83.65(4) 3_576 . ?
N1 Y1 C10 100.72(4) . . ?
N1 Y1 C10 120.95(4) 3_576 . ?
O1 Y1 C10 126.80(4) . . ?
N1 Y1 C9 127.82(4) . . ?
N1 Y1 C9 135.43(4) 3_576 . ?
O1 Y1 C9 97.41(4) . . ?
C10 Y1 C9 31.00(4) . . ?
N1 Y1 C3 129.50(4) . . ?
N1 Y1 C3 131.47(4) 3_576 . ?
O1 Y1 C3 82.99(4) . . ?
C10 Y1 C3 104.19(5) . . ?
C9 Y1 C3 92.54(5) . . ?
N1 Y1 C2 103.08(4) . . ?
N1 Y1 C2 100.83(4) 3_576 . ?
O1 Y1 C2 79.29(4) . . ?
C10 Y1 C2 130.70(4) . . ?
C9 Y1 C2 123.27(5) . . ?
C3 Y1 C2 30.75(5) . . ?
N1 Y1 C11 76.87(4) . . ?
N1 Y1 C11 90.91(4) 3_576 . ?
O1 Y1 C11 122.30(4) . . ?
C10 Y1 C11 30.79(4) . . ?
C9 Y1 C11 51.01(4) . . ?
C3 Y1 C11 134.85(4) . . ?
C2 Y1 C11 156.75(4) . . ?
N1 Y1 C4 117.60(4) . . ?
N1 Y1 C4 139.16(4) 3_576 . ?
O1 Y1 C4 112.76(4) . . ?
C10 Y1 C4 80.06(4) . . ?
C9 Y1 C4 81.40(4) . . ?
C3 Y1 C4 30.76(4) . . ?
C2 Y1 C4 50.66(4) . . ?
C11 Y1 C4 108.23(4) . . ?
N1 Y1 C1 78.99(4) . . ?
N1 Y1 C1 89.81(4) 3_576 . ?
O1 Y1 C1 106.30(4) . . ?
C10 Y1 C1 118.83(5) . . ?
C9 Y1 C1 131.25(4) . . ?
C3 Y1 C1 50.52(5) . . ?
C2 Y1 C1 30.53(5) . . ?
C11 Y1 C1 131.16(5) . . ?
C4 Y1 C1 50.31(4) . . ?
N1 Y1 C7 86.85(4) . . ?
N1 Y1 C7 84.84(4) 3_576 . ?
O1 Y1 C7 91.80(4) . . ?
C10 Y1 C7 50.58(4) . . ?
C9 Y1 C7 50.61(4) . . ?
C3 Y1 C7 141.93(4) . . ?
C2 Y1 C7 168.74(5) . . ?
C11 Y1 C7 30.59(4) . . ?
C4 Y1 C7 129.12(4) . . ?
C1 Y1 C7 160.46(5) . . ?
N1 Y1 C8 117.37(4) . . ?
N1 Y1 C8 109.70(4) 3_576 . ?
O1 Y1 C8 77.49(4) . . ?
C10 Y1 C8 50.67(4) . . ?
C9 Y1 C8 30.52(4) . . ?
C3 Y1 C8 112.45(5) . . ?
C2 Y1 C8 138.89(5) . . ?
C11 Y1 C8 50.70(4) . . ?
C4 Y1 C8 110.31(4) . . ?
C1 Y1 C8 160.48(4) . . ?
C7 Y1 C8 30.59(4) . . ?
C16 O1 C13 109.29(10) . . ?
C16 O1 Y1 127.91(8) . . ?
C13 O1 Y1 122.44(8) . . ?
N1 N1 Y1 75.54(10) 3_576 . ?
N1 N1 Y1 73.17(10) 3_576 3_576 ?
Y1 N1 Y1 148.70(5) . 3_576 ?
C2 C1 C5 108.97(13) . . ?
C2 C1 Y1 74.40(8) . . ?
C5 C1 Y1 75.09(8) . . ?
C1 C2 C3 107.70(13) . . ?
C1 C2 Y1 75.06(8) . . ?
C3 C2 Y1 74.33(8) . . ?
C2 C3 C4 107.84(13) . . ?
C2 C3 Y1 74.91(8) . . ?
C4 C3 Y1 75.17(8) . . ?
C5 C4 C3 108.65(13) . . ?
C5 C4 Y1 75.20(8) . . ?
C3 C4 Y1 74.06(8) . . ?
C4 C5 C1 106.84(13) . . ?
C4 C5 C6 127.20(13) . . ?
C1 C5 C6 125.93(13) . . ?
C4 C5 Y1 74.22(8) . . ?
C1 C5 Y1 74.24(8) . . ?
C6 C5 Y1 118.74(9) . . ?
C11 C7 C8 108.55(12) . . ?
C11 C7 Y1 74.58(8) . . ?
C8 C7 Y1 75.00(8) . . ?
C9 C8 C7 107.93(13) . . ?
C9 C8 Y1 73.76(8) . . ?
C7 C8 Y1 74.40(8) . . ?
C8 C9 C10 107.71(12) . . ?
C8 C9 Y1 75.73(8) . . ?
C10 C9 Y1 73.86(8) . . ?
C11 C10 C9 108.55(12) . . ?
C11 C10 Y1 75.80(8) . . ?
C9 C10 Y1 75.14(8) . . ?
C7 C11 C10 107.25(12) . . ?
C7 C11 C12 127.14(13) . . ?
C10 C11 C12 125.53(13) . . ?
C7 C11 Y1 74.83(8) . . ?
C10 C11 Y1 73.41(8) . . ?
C12 C11 Y1 119.83(9) . . ?
O1 C13 C14 104.31(11) . . ?
C13 C14 C15 102.43(12) . . ?
C16 C15 C14 102.18(12) . . ?
O1 C16 C15 106.22(11) . . ?

_refine_diff_density_max         0.387
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054

_shelxl_version_number           2014-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dhw15
_database_code_depnum_ccdc_archive 'CCDC 1415200'
_audit_update_record             
;
2015-07-26 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[(C5H4Me)2Dy]2(μ-η2:η2-N2)'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 Dy2 N2 O2'
_chemical_formula_weight         813.69

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.9046(7)
_cell_length_b                   10.0279(6)
_cell_length_c                   12.7468(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.7793(8)
_cell_angle_gamma                90
_cell_volume                     1513.95(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9880
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.70

_exptl_crystal_description       irregular
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             796
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.169
_exptl_absorpt_coefficient_mu    4.927
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2979
_exptl_absorpt_correction_T_max  0.4316
_exptl_absorpt_process_details   'Bruker TWINABS 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3608
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.231
_diffrn_reflns_theta_max         28.730
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3608
_reflns_number_gt                3406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.9-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
A green crystal of approximate dimensions 0.169 x 0.199 x 0.265 mm was mounted
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer. The
APEX2 program package and the CELL_NOW were used to determine the unit-cell
parameters.  Data was collected using a 10 sec/frame scan time for a sphere of
diffraction data.  The raw frame data was processed using SAINT and TWINABS to
yield the reflection data file (HKLF 5 format).  Subsequent calculations were
carried out using the SHELXTL program.  The diffraction symmetry was 2/m and the
systematic absences were consistent with the monoclinic space group P21/n that
was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix
least-squares techniques.  The analytical scattering factors for neutral atoms were
used throughout the analysis.  Hydrogen atoms were included using a riding model.
The molecule was located about an inversion center (Z = 2).

At convergence, wR2 = 0.0403 and Goof = 1.036 for 175 variables refined against 3608
data (0.74), R1 = 0.0164 for those 3406 with I > 2.0sigma(I).  The structure was
refined as a two-component twin, BASF5 = 0.4066.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+0.4971P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3608
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0396
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.32205(2) 0.43061(2) 0.49918(2) 0.01089(4) Uani 1 1 d . . . . .
O1 O 0.23053(14) 0.64501(17) 0.50575(14) 0.0173(4) Uani 1 1 d . . . . .
N1 N 0.51504(17) 0.44027(19) 0.50261(16) 0.0133(4) Uani 1 1 d . . . . .
C1 C 0.3845(2) 0.3608(3) 0.6996(2) 0.0223(6) Uani 1 1 d . . . . .
H1A H 0.4603 0.3788 0.7383 0.027 Uiso 1 1 calc R U . . .
C2 C 0.2895(3) 0.4415(3) 0.7034(2) 0.0237(7) Uani 1 1 d . . . . .
H2A H 0.2859 0.5248 0.7461 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1954(2) 0.3715(3) 0.6534(2) 0.0215(6) Uani 1 1 d . . . . .
H3A H 0.1144 0.3970 0.6554 0.026 Uiso 1 1 calc R U . . .
C4 C 0.2345(2) 0.2472(3) 0.6196(2) 0.0178(5) Uani 1 1 d . . . . .
H4A H 0.1853 0.1712 0.5929 0.021 Uiso 1 1 calc R U . . .
C5 C 0.3525(2) 0.2397(3) 0.6473(2) 0.0183(5) Uani 1 1 d . . . . .
C6 C 0.4288(2) 0.1245(3) 0.6296(2) 0.0251(6) Uani 1 1 d . . . . .
H6A H 0.4101 0.0490 0.6734 0.038 Uiso 1 1 calc R U . . .
H6B H 0.5075 0.1509 0.6486 0.038 Uiso 1 1 calc R U . . .
H6C H 0.4186 0.0985 0.5551 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3143(2) 0.4419(3) 0.28875(19) 0.0149(5) Uani 1 1 d . . . . .
H7A H 0.3513 0.5119 0.2482 0.018 Uiso 1 1 calc R U . . .
C8 C 0.2006(2) 0.4433(3) 0.3100(2) 0.0209(6) Uani 1 1 d . . . . .
H8A H 0.1440 0.5137 0.2869 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1765(2) 0.3189(3) 0.3530(2) 0.0212(6) Uani 1 1 d . . . . .
H9A H 0.0995 0.2853 0.3644 0.025 Uiso 1 1 calc R U . . .
C10 C 0.2761(2) 0.2405(3) 0.3575(2) 0.0185(5) Uani 1 1 d . . . . .
H10A H 0.2802 0.1426 0.3724 0.022 Uiso 1 1 calc R U . . .
C11 C 0.3612(2) 0.3160(3) 0.31669(19) 0.0158(5) Uani 1 1 d . . . . .
C12 C 0.4773(2) 0.2682(3) 0.3006(2) 0.0263(6) Uani 1 1 d . . . . .
H12A H 0.4769 0.2294 0.2300 0.040 Uiso 1 1 calc R U . . .
H12B H 0.5011 0.2005 0.3536 0.040 Uiso 1 1 calc R U . . .
H12C H 0.5301 0.3435 0.3076 0.040 Uiso 1 1 calc R U . . .
C13 C 0.2729(2) 0.7640(2) 0.4567(2) 0.0198(5) Uani 1 1 d . . . . .
H13A H 0.2574 0.7598 0.3790 0.024 Uiso 1 1 calc R U . . .
H13B H 0.3552 0.7741 0.4753 0.024 Uiso 1 1 calc R U . . .
C14 C 0.2089(2) 0.8773(3) 0.5012(2) 0.0243(6) Uani 1 1 d . . . . .
H14A H 0.2041 0.9552 0.4532 0.029 Uiso 1 1 calc R U . . .
H14B H 0.2448 0.9051 0.5712 0.029 Uiso 1 1 calc R U . . .
C15 C 0.0935(2) 0.8167(3) 0.5094(2) 0.0252(6) Uani 1 1 d . . . . .
H15A H 0.0471 0.8174 0.4404 0.030 Uiso 1 1 calc R U . . .
H15B H 0.0526 0.8645 0.5619 0.030 Uiso 1 1 calc R U . . .
C16 C 0.1231(2) 0.6754(3) 0.5450(3) 0.0265(6) Uani 1 1 d . . . . .
H16A H 0.1297 0.6693 0.6229 0.032 Uiso 1 1 calc R U . . .
H16B H 0.0643 0.6121 0.5157 0.032 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Dy1 Cnt1 2.391 . ?
Dy1 Cnt2 2.385 . ?
Dy1 N1 2.296(2) . ?
Dy1 N1 2.334(2) 3_666 ?
Dy1 O1 2.4156(17) . ?
Dy1 C10 2.645(2) . ?
Dy1 C9 2.661(3) . ?
Dy1 C3 2.662(3) . ?
Dy1 C2 2.673(3) . ?
Dy1 C4 2.674(2) . ?
Dy1 C7 2.677(2) . ?
Dy1 C11 2.677(2) . ?
Dy1 C1 2.681(3) . ?
Dy1 C8 2.686(3) . ?
O1 C16 1.451(3) . ?
O1 C13 1.460(3) . ?
N1 N1 1.250(4) 3_666 ?
N1 Dy1 2.334(2) 3_666 ?
C1 C2 1.395(4) . ?
C1 C5 1.420(4) . ?
C2 C3 1.419(4) . ?
C3 C4 1.412(4) . ?
C4 C5 1.415(4) . ?
C5 C6 1.500(4) . ?
C7 C8 1.407(4) . ?
C7 C11 1.411(4) . ?
C8 C9 1.404(4) . ?
C9 C10 1.419(4) . ?
C10 C11 1.405(4) . ?
C11 C12 1.497(4) . ?
C13 C14 1.510(4) . ?
C14 C15 1.516(4) . ?
C15 C16 1.520(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
Cnt1 Dy1 N1 104.0 . . ?
Cnt1 Dy1 N1 116.0 . 3_666 ?
Cnt1 Dy1 O1 103.1 . . ?
Cnt2 Dy1 N1 102.6 . . ?
Cnt2 Dy1 N1 109.3 . 3_666 ?
Cnt2 Dy1 O1 103.9 . . ?
Cnt1 Dy1 Cnt2 129.1 . . ?
N1 Dy1 N1 31.32(9) . 3_666 ?
N1 Dy1 O1 114.57(6) . . ?
N1 Dy1 O1 83.38(6) 3_666 . ?
N1 Dy1 C10 100.44(8) . . ?
N1 Dy1 C10 120.54(8) 3_666 . ?
O1 Dy1 C10 127.02(8) . . ?
N1 Dy1 C9 127.68(8) . . ?
N1 Dy1 C9 135.25(8) 3_666 . ?
O1 Dy1 C9 97.75(8) . . ?
C10 Dy1 C9 31.02(8) . . ?
N1 Dy1 C3 129.47(8) . . ?
N1 Dy1 C3 131.60(8) 3_666 . ?
O1 Dy1 C3 83.21(7) . . ?
C10 Dy1 C3 104.47(9) . . ?
C9 Dy1 C3 92.61(9) . . ?
N1 Dy1 C2 102.86(9) . . ?
N1 Dy1 C2 100.88(8) 3_666 . ?
O1 Dy1 C2 79.62(8) . . ?
C10 Dy1 C2 130.87(8) . . ?
C9 Dy1 C2 123.45(9) . . ?
C3 Dy1 C2 30.85(9) . . ?
N1 Dy1 C4 117.74(8) . . ?
N1 Dy1 C4 139.43(8) 3_666 . ?
O1 Dy1 C4 112.89(7) . . ?
C10 Dy1 C4 80.24(8) . . ?
C9 Dy1 C4 81.27(8) . . ?
C3 Dy1 C4 30.69(8) . . ?
C2 Dy1 C4 50.63(8) . . ?
N1 Dy1 C7 87.17(8) . . ?
N1 Dy1 C7 84.93(8) 3_666 . ?
O1 Dy1 C7 91.55(7) . . ?
C10 Dy1 C7 50.38(8) . . ?
C9 Dy1 C7 50.36(8) . . ?
C3 Dy1 C7 141.66(9) . . ?
C2 Dy1 C7 168.70(9) . . ?
C4 Dy1 C7 128.93(8) . . ?
N1 Dy1 C11 76.90(8) . . ?
N1 Dy1 C11 90.71(8) 3_666 . ?
O1 Dy1 C11 122.06(7) . . ?
C10 Dy1 C11 30.61(8) . . ?
C9 Dy1 C11 50.86(8) . . ?
C3 Dy1 C11 134.98(8) . . ?
C2 Dy1 C11 156.76(8) . . ?
C4 Dy1 C11 108.39(8) . . ?
C7 Dy1 C11 30.57(8) . . ?
N1 Dy1 C1 79.15(8) . . ?
N1 Dy1 C1 90.17(8) 3_666 . ?
O1 Dy1 C1 106.38(8) . . ?
C10 Dy1 C1 118.76(9) . . ?
C9 Dy1 C1 130.99(8) . . ?
C3 Dy1 C1 50.33(9) . . ?
C2 Dy1 C1 30.21(9) . . ?
C4 Dy1 C1 50.21(8) . . ?
C7 Dy1 C1 160.75(9) . . ?
C11 Dy1 C1 131.31(9) . . ?
N1 Dy1 C8 117.53(8) . . ?
N1 Dy1 C8 109.73(8) 3_666 . ?
O1 Dy1 C8 77.60(7) . . ?
C10 Dy1 C8 50.63(8) . . ?
C9 Dy1 C8 30.44(8) . . ?
C3 Dy1 C8 112.31(9) . . ?
C2 Dy1 C8 139.00(10) . . ?
C4 Dy1 C8 110.01(8) . . ?
C7 Dy1 C8 30.42(8) . . ?
C11 Dy1 C8 50.61(8) . . ?
C1 Dy1 C8 160.09(9) . . ?
C16 O1 C13 109.31(18) . . ?
C16 O1 Dy1 127.92(14) . . ?
C13 O1 Dy1 122.40(14) . . ?
N1 N1 Dy1 76.03(18) 3_666 . ?
N1 N1 Dy1 72.65(17) 3_666 3_666 ?
Dy1 N1 Dy1 148.68(9) . 3_666 ?
C2 C1 C5 109.4(3) . . ?
C2 C1 Dy1 74.56(15) . . ?
C5 C1 Dy1 74.90(15) . . ?
C1 C2 C3 107.7(2) . . ?
C1 C2 Dy1 75.23(15) . . ?
C3 C2 Dy1 74.15(15) . . ?
C4 C3 C2 107.7(3) . . ?
C4 C3 Dy1 75.13(14) . . ?
C2 C3 Dy1 75.00(15) . . ?
C3 C4 C5 108.7(2) . . ?
C3 C4 Dy1 74.18(14) . . ?
C5 C4 Dy1 75.21(14) . . ?
C4 C5 C1 106.6(2) . . ?
C4 C5 C6 127.2(2) . . ?
C1 C5 C6 126.2(3) . . ?
C4 C5 Dy1 74.17(14) . . ?
C1 C5 Dy1 74.43(15) . . ?
C6 C5 Dy1 118.91(17) . . ?
C8 C7 C11 108.9(2) . . ?
C8 C7 Dy1 75.15(15) . . ?
C11 C7 Dy1 74.72(14) . . ?
C9 C8 C7 107.8(2) . . ?
C9 C8 Dy1 73.77(15) . . ?
C7 C8 Dy1 74.43(15) . . ?
C8 C9 C10 107.7(2) . . ?
C8 C9 Dy1 75.78(15) . . ?
C10 C9 Dy1 73.86(15) . . ?
C11 C10 C9 108.5(2) . . ?
C11 C10 Dy1 75.97(14) . . ?
C9 C10 Dy1 75.11(14) . . ?
C10 C11 C7 107.1(2) . . ?
C10 C11 C12 126.1(2) . . ?
C7 C11 C12 126.8(2) . . ?
C10 C11 Dy1 73.42(14) . . ?
C7 C11 Dy1 74.71(14) . . ?
C12 C11 Dy1 120.03(17) . . ?
O1 C13 C14 104.2(2) . . ?
C13 C14 C15 102.7(2) . . ?
C14 C15 C16 102.1(2) . . ?
O1 C16 C15 106.2(2) . . ?

_refine_diff_density_max         1.022
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.097

