#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:45:35 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236999 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/77/4087781.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4087781
loop_
_publ_author_name
'Schädle, Dorothea'
'Schädle, Christoph'
'Schneider, David'
'Maichle-Mössmer, Cäcilia'
'Anwander, Reiner'
_publ_section_title
;
 Versatile Ln2(μ-NR)2-Imide Platforms for Ligand Exchange and Isoprene
 Polymerization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4994
_journal_paper_doi               10.1021/acs.organomet.5b00589
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C62 H96 La2 N6 Si2'
_chemical_formula_sum            'C62 H96 La2 N6 Si2'
_chemical_formula_weight         1259.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.0030(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3792(2)
_cell_length_b                   13.3141(2)
_cell_length_c                   18.8022(3)
_cell_measurement_reflns_used    945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1341
_cell_measurement_theta_min      3.0068
_cell_volume                     3060.76(8)
_computing_cell_refinement       'APEX2 v2013.6-2 (Bruker AXS)'
_computing_data_collection       'COSMO v1.61'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Ortep3, POV-Ray'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'APEX II DUO'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation.monochromator  'multilayer QUAZAR'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0228P)²+1.9331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6065
_reflns_number_total             6751
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00589_si_002.cif
_cod_data_source_block           Compound_10-La
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087781
_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.
;
_shelx_estimated_absorpt_t_min   0.661
_shelx_estimated_absorpt_t_max   0.863
_shelxl_version_number           2013-3
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'
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
La1 La 0.62653(2) 0.93011(2) 0.51104(2) 0.01200(4) Uani 1 1 d . U
Si1 Si 0.79944(4) 0.62686(4) 0.51979(3) 0.01708(10) Uani 1 1 d . U
N1 N 0.45558(12) 0.92897(10) 0.55020(8) 0.0143(3) Uani 1 1 d . U
N2 N 0.79798(12) 0.97287(12) 0.61514(8) 0.0213(3) Uani 1 1 d . U
N3 N 1.06209(13) 0.95209(13) 0.78419(9) 0.0235(3) Uani 1 1 d . U
C1 C 0.71396(13) 0.73046(13) 0.47298(9) 0.0150(3) Uani 1 1 d . U
C2 C 0.59643(13) 0.73135(13) 0.45504(9) 0.0153(3) Uani 1 1 d . U
C3 C 0.56664(14) 0.79740(13) 0.39668(9) 0.0164(3) Uani 1 1 d . U
C4 C 0.66349(14) 0.84087(13) 0.37802(9) 0.0167(3) Uani 1 1 d . U
C5 C 0.75306(13) 0.79911(13) 0.42369(9) 0.0157(3) Uani 1 1 d . U
C6 C 0.51547(15) 0.67493(14) 0.49252(11) 0.0222(4) Uani 1 1 d . U
H6A H 0.4424 0.7039 0.4788 0.033 Uiso 1 1 calc R U
H6B H 0.5372 0.6803 0.5448 0.033 Uiso 1 1 calc R U
H6C H 0.5143 0.6041 0.4783 0.033 Uiso 1 1 calc R U
C7 C 0.45287(15) 0.81622(15) 0.35710(11) 0.0244(4) Uani 1 1 d . U
H7A H 0.4475 0.8855 0.3393 0.037 Uiso 1 1 calc R U
H7B H 0.3997 0.8057 0.3899 0.037 Uiso 1 1 calc R U
H7C H 0.4375 0.7697 0.3164 0.037 Uiso 1 1 calc R U
C8 C 0.66747(17) 0.91395(14) 0.31727(10) 0.0240(4) Uani 1 1 d . U
H8A H 0.6373 0.8821 0.2715 0.036 Uiso 1 1 calc R U
H8B H 0.7435 0.9337 0.3162 0.036 Uiso 1 1 calc R U
H8C H 0.6242 0.9736 0.3246 0.036 Uiso 1 1 calc R U
C9 C 0.87161(14) 0.81513(14) 0.41530(10) 0.0210(4) Uani 1 1 d . U
H9A H 0.8899 0.7719 0.3767 0.032 Uiso 1 1 calc R U
H9B H 0.9188 0.7983 0.4606 0.032 Uiso 1 1 calc R U
H9C H 0.8828 0.8856 0.4032 0.032 Uiso 1 1 calc R U
C10 C 0.85975(16) 0.55012(15) 0.45151(11) 0.0262(4) Uani 1 1 d . U
H10A H 0.8007 0.5214 0.4167 0.039 Uiso 1 1 calc R U
H10B H 0.9043 0.4958 0.4760 0.039 Uiso 1 1 calc R U
H10C H 0.9056 0.5932 0.4263 0.039 Uiso 1 1 calc R U
C11 C 0.91844(15) 0.66445(15) 0.58939(11) 0.0253(4) Uani 1 1 d . U
H11A H 0.9664 0.7097 0.5676 0.038 Uiso 1 1 calc R U
H11B H 0.9595 0.6044 0.6076 0.038 Uiso 1 1 calc R U
H11C H 0.8915 0.6988 0.6292 0.038 Uiso 1 1 calc R U
C12 C 0.41470(14) 0.86173(13) 0.59586(9) 0.0157(3) Uani 1 1 d . U
C13 C 0.47255(15) 0.83711(14) 0.66594(10) 0.0208(4) Uani 1 1 d . U
C14 C 0.42807(17) 0.77185(17) 0.71121(12) 0.0309(5) Uani 1 1 d . U
H14 H 0.4679 0.7581 0.7576 0.037 Uiso 1 1 calc R U
C15 C 0.32732(18) 0.72617(18) 0.69077(13) 0.0395(6) Uani 1 1 d . U
H15 H 0.2982 0.6816 0.7224 0.047 Uiso 1 1 calc R U
C16 C 0.27049(16) 0.74719(16) 0.62333(13) 0.0327(5) Uani 1 1 d . U
H16 H 0.2015 0.7161 0.6088 0.039 Uiso 1 1 calc R U
C17 C 0.31079(14) 0.81255(14) 0.57579(11) 0.0212(4) Uani 1 1 d . U
C18 C 0.58499(16) 0.88025(15) 0.69293(10) 0.0219(4) Uani 1 1 d . U
H18 H 0.5988 0.9347 0.6589 0.026 Uiso 1 1 calc R U
C19 C 0.67389(16) 0.79997(15) 0.69163(12) 0.0305(5) Uani 1 1 d . U
H19A H 0.6701 0.7738 0.6426 0.046 Uiso 1 1 calc R U
H19B H 0.6622 0.7450 0.7242 0.046 Uiso 1 1 calc R U
H19C H 0.7460 0.8299 0.7072 0.046 Uiso 1 1 calc R U
C20 C 0.5953(2) 0.92681(18) 0.76813(11) 0.0375(5) Uani 1 1 d . U
H20A H 0.6668 0.9594 0.7801 0.056 Uiso 1 1 calc R U
H20B H 0.5884 0.8741 0.8035 0.056 Uiso 1 1 calc R U
H20C H 0.5373 0.9767 0.7689 0.056 Uiso 1 1 calc R U
C21 C 0.23878(14) 0.83663(14) 0.50523(11) 0.0215(4) Uani 1 1 d . U
H21 H 0.2845 0.8733 0.4743 0.026 Uiso 1 1 calc R U
C22 C 0.14664(16) 0.90767(16) 0.51939(12) 0.0280(4) Uani 1 1 d . U
H22A H 0.1016 0.9256 0.4736 0.042 Uiso 1 1 calc R U
H22B H 0.1784 0.9687 0.5432 0.042 Uiso 1 1 calc R U
H22C H 0.1011 0.8741 0.5504 0.042 Uiso 1 1 calc R U
C23 C 0.18983(17) 0.74503(17) 0.46307(14) 0.0353(5) Uani 1 1 d . U
H23A H 0.1499 0.7667 0.4165 0.053 Uiso 1 1 calc R U
H23B H 0.1396 0.7107 0.4904 0.053 Uiso 1 1 calc R U
H23C H 0.2486 0.6990 0.4553 0.053 Uiso 1 1 calc R U
C24 C 0.71831(16) 0.53801(15) 0.56758(11) 0.0266(4) Uani 1 1 d . U
H24A H 0.6603 0.5076 0.5328 0.040 Uiso 1 1 calc R U
H24B H 0.6856 0.5747 0.6041 0.040 Uiso 1 1 calc R U
H24C H 0.7665 0.4852 0.5909 0.040 Uiso 1 1 calc R U
C25 C 0.80527(15) 1.03030(15) 0.67449(10) 0.0225(4) Uani 1 1 d . U
H25 H 0.7472 1.0759 0.6777 0.027 Uiso 1 1 calc R U
C26 C 0.89079(15) 1.02778(15) 0.73094(10) 0.0222(4) Uani 1 1 d . U
H26 H 0.8902 1.0705 0.7713 0.027 Uiso 1 1 calc R U
C27 C 0.97933(14) 0.96163(14) 0.72877(10) 0.0194(4) Uani 1 1 d . U
C28 C 0.97461(15) 0.90500(15) 0.66517(10) 0.0223(4) Uani 1 1 d . U
H28 H 1.0332 0.8615 0.6588 0.027 Uiso 1 1 calc R U
C29 C 0.88496(16) 0.91291(15) 0.61242(11) 0.0244(4) Uani 1 1 d . U
H29 H 0.8841 0.8728 0.5705 0.029 Uiso 1 1 calc R U
C30 C 1.15245(16) 0.88358(17) 0.77929(11) 0.0294(5) Uani 1 1 d . U
H30A H 1.1240 0.8154 0.7700 0.044 Uiso 1 1 calc R U
H30B H 1.2036 0.8846 0.8247 0.044 Uiso 1 1 calc R U
H30C H 1.1905 0.9047 0.7399 0.044 Uiso 1 1 calc R U
C31 C 1.05476(17) 0.99917(18) 0.85306(11) 0.0317(5) Uani 1 1 d . U
H31A H 1.0614 1.0722 0.8486 0.047 Uiso 1 1 calc R U
H31B H 1.1139 0.9742 0.8896 0.047 Uiso 1 1 calc R U
H31C H 0.9840 0.9829 0.8674 0.047 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 La1 N1 79.44(5) . 3_676
N1 La1 N2 114.65(5) . .
N1 La1 N2 114.58(5) 3_676 .
N1 La1 C3 95.38(5) . .
N1 La1 C3 94.91(5) 3_676 .
N2 La1 C3 140.52(5) . .
N1 La1 C2 92.16(5) . .
N1 La1 C2 122.62(5) 3_676 .
N2 La1 C2 120.23(5) . .
C3 La1 C2 28.90(5) . .
N1 La1 C4 123.05(5) . .
N1 La1 C4 91.10(5) 3_676 .
N2 La1 C4 120.15(5) . .
C3 La1 C4 29.09(5) . .
C2 La1 C4 47.41(5) . .
N1 La1 C1 116.48(5) . .
N1 La1 C1 137.40(5) 3_676 .
N2 La1 C1 95.01(5) . .
C3 La1 C1 46.96(5) . .
C2 La1 C1 28.38(4) . .
C4 La1 C1 46.55(5) . .
N1 La1 C5 137.88(5) . .
N1 La1 C5 114.78(5) 3_676 .
N2 La1 C5 95.76(5) . .
C3 La1 C5 46.28(5) . .
C2 La1 C5 46.16(5) . .
C4 La1 C5 27.61(5) . .
C1 La1 C5 27.75(5) . .
N1 La1 La1 39.73(3) . 3_676
N1 La1 La1 39.71(3) 3_676 3_676
N2 La1 La1 122.78(3) . 3_676
C3 La1 La1 96.69(3) . 3_676
C2 La1 La1 112.02(3) . 3_676
C4 La1 La1 111.53(3) . 3_676
C1 La1 La1 140.21(3) . 3_676
C5 La1 La1 138.99(3) . 3_676
C24 Si1 C1 112.66(8) . .
C24 Si1 C11 104.79(9) . .
C1 Si1 C11 117.07(8) . .
C24 Si1 C10 106.52(10) . .
C1 Si1 C10 109.53(8) . .
C11 Si1 C10 105.54(9) . .
C12 N1 La1 129.16(11) . .
C12 N1 La1 130.26(11) . 3_676
La1 N1 La1 100.56(5) . 3_676
C25 N2 C29 114.72(15) . .
C25 N2 La1 131.43(12) . .
C29 N2 La1 112.82(12) . .
C27 N3 C31 120.12(16) . .
C27 N3 C30 120.53(16) . .
C31 N3 C30 118.79(16) . .
C5 C1 C2 105.85(14) . .
C5 C1 Si1 123.27(12) . .
C2 C1 Si1 126.28(13) . .
C5 C1 La1 76.17(9) . .
C2 C1 La1 70.10(9) . .
Si1 C1 La1 137.69(8) . .
C3 C2 C1 108.60(15) . .
C3 C2 C6 124.12(15) . .
C1 C2 C6 127.25(16) . .
C3 C2 La1 73.24(10) . .
C1 C2 La1 81.52(10) . .
C6 C2 La1 110.30(11) . .
C2 C3 C4 108.52(15) . .
C2 C3 C7 126.76(16) . .
C4 C3 C7 124.64(16) . .
C2 C3 La1 77.86(10) . .
C4 C3 La1 78.47(10) . .
C7 C3 La1 112.95(11) . .
C5 C4 C3 107.62(15) . .
C5 C4 C8 126.99(16) . .
C3 C4 C8 125.31(16) . .
C5 C4 La1 81.35(10) . .
C3 C4 La1 72.44(9) . .
C8 C4 La1 114.95(11) . .
C4 C5 C1 109.38(15) . .
C4 C5 C9 124.38(16) . .
C1 C5 C9 125.84(15) . .
C4 C5 La1 71.04(9) . .
C1 C5 La1 76.08(9) . .
C9 C5 La1 124.91(11) . .
N1 C12 C13 122.45(16) . .
N1 C12 C17 121.86(16) . .
C13 C12 C17 115.69(16) . .
C14 C13 C12 121.11(18) . .
C14 C13 C18 117.55(17) . .
C12 C13 C18 121.34(16) . .
C15 C14 C13 122.0(2) . .
C16 C15 C14 118.24(19) . .
C15 C16 C17 122.3(2) . .
C16 C17 C12 120.68(18) . .
C16 C17 C21 118.27(17) . .
C12 C17 C21 120.88(16) . .
C13 C18 C20 113.68(17) . .
C13 C18 C19 110.67(16) . .
C20 C18 C19 109.87(17) . .
C17 C21 C23 114.68(17) . .
C17 C21 C22 109.27(16) . .
C23 C21 C22 109.66(16) . .
N2 C25 C26 124.72(17) . .
C25 C26 C27 119.98(17) . .
N3 C27 C28 122.13(17) . .
N3 C27 C26 122.42(17) . .
C28 C27 C26 115.45(16) . .
C29 C28 C27 119.64(17) . .
N2 C29 C28 125.36(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 N1 2.3469(14) .
La1 N1 2.3480(14) 3_676
La1 N2 2.7129(15) .
La1 C3 2.7922(17) .
La1 C2 2.8509(17) .
La1 C4 2.8697(17) .
La1 C1 2.9987(17) .
La1 C5 2.9998(16) .
La1 La1 3.61131(18) 3_676
Si1 C24 1.870(2) .
Si1 C1 1.8723(17) .
Si1 C11 1.8788(19) .
Si1 C10 1.884(2) .
N1 C12 1.389(2) .
N1 La1 2.3480(14) 3_676
N2 C25 1.344(2) .
N2 C29 1.348(2) .
N3 C27 1.348(2) .
N3 C31 1.454(3) .
N3 C30 1.457(3) .
C1 C5 1.438(2) .
C1 C2 1.441(2) .
C2 C3 1.409(2) .
C2 C6 1.512(2) .
C3 C4 1.424(2) .
C3 C7 1.507(2) .
C4 C5 1.406(2) .
C4 C8 1.507(3) .
C5 C9 1.515(2) .
C12 C13 1.436(3) .
C12 C17 1.440(2) .
C13 C14 1.389(3) .
C13 C18 1.518(3) .
C14 C15 1.387(3) .
C15 C16 1.379(3) .
C16 C17 1.395(3) .
C17 C21 1.512(3) .
C18 C20 1.531(3) .
C18 C19 1.537(3) .
C21 C23 1.527(3) .
C21 C22 1.537(3) .
C25 C26 1.377(3) .
C26 C27 1.412(3) .
C27 C28 1.407(3) .
C28 C29 1.372(3) .
