#------------------------------------------------------------------------------
#$Date: 2015-12-06 11:00:56 +0200 (Sun, 06 Dec 2015) $
#$Revision: 170843 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/06/1540639.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_1540639
loop_
_publ_author_name
'Sroor, Farid'
'Hrib, Cristian'
'Edelmann, Frank'
_publ_section_title
;
 New Lanthanide Alkynylamidinates and Diiminophosphinates
;
_journal_issue                   4
_journal_name_full               Inorganics
_journal_page_first              429
_journal_paper_doi               10.3390/inorganics3040429
_journal_volume                  3
_journal_year                    2015
_chemical_formula_sum            'C50 H70 Li2 N4 O2'
_chemical_formula_weight         772.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.144(3)
_cell_angle_beta                 90.248(3)
_cell_angle_gamma                104.209(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8768(3)
_cell_length_b                   10.2082(3)
_cell_length_c                   11.6883(4)
_cell_measurement_reflns_used    29727
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.8730
_cell_measurement_theta_min      3.8970
_cell_volume                     1105.18(6)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40575
_diffrn_reflns_theta_full        76.97
_diffrn_reflns_theta_max         76.97
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.9392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.4073P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                4442
_reflns_number_total             4628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            magd78.cif
_cod_data_source_block           magd78
_cod_database_code               1540639
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O O 0.06968(9) 0.27453(9) 1.09079(8) 0.0327(2) Uani 1 1 d .
N1 N 0.25156(9) 0.58320(9) 1.01094(7) 0.02038(18) Uani 1 1 d .
N2 N 0.07581(8) 0.46646(8) 0.86677(7) 0.01848(18) Uani 1 1 d .
C1 C 0.20890(10) 0.53952(10) 0.89770(8) 0.01725(19) Uani 1 1 d .
C2 C 0.30430(10) 0.57459(10) 0.80750(8) 0.0184(2) Uani 1 1 d .
C3 C 0.38565(10) 0.61255(10) 0.73885(9) 0.0191(2) Uani 1 1 d .
C4 C 0.48575(10) 0.66055(10) 0.65975(8) 0.0189(2) Uani 1 1 d .
C5 C 0.59371(11) 0.59552(11) 0.62594(9) 0.0239(2) Uani 1 1 d .
H5 H 0.6009 0.5179 0.6547 0.029 Uiso 1 1 calc R
C6 C 0.69041(11) 0.64446(12) 0.55028(10) 0.0279(2) Uani 1 1 d .
H6 H 0.7632 0.5996 0.5269 0.033 Uiso 1 1 calc R
C7 C 0.68130(11) 0.75808(12) 0.50883(9) 0.0291(2) Uani 1 1 d .
H7 H 0.7484 0.7918 0.4579 0.035 Uiso 1 1 calc R
C8 C 0.57426(12) 0.82282(12) 0.54154(10) 0.0293(2) Uani 1 1 d .
H8 H 0.5679 0.9006 0.5127 0.035 Uiso 1 1 calc R
C9 C 0.47644(11) 0.77426(11) 0.61628(9) 0.0235(2) Uani 1 1 d .
H9 H 0.4029 0.8185 0.6380 0.028 Uiso 1 1 calc R
C10 C 0.39053(10) 0.67577(10) 1.04741(8) 0.0193(2) Uani 1 1 d .
H10 H 0.4515 0.6613 0.9798 0.023 Uiso 1 1 calc R
C11 C 0.38697(11) 0.82943(11) 1.08163(9) 0.0227(2) Uani 1 1 d .
H11A H 0.3491 0.8531 1.0129 0.027 Uiso 1 1 calc R
H11B H 0.3237 0.8443 1.1463 0.027 Uiso 1 1 calc R
C12 C 0.53281(11) 0.92609(11) 1.12184(10) 0.0245(2) Uani 1 1 d .
H12A H 0.5260 1.0240 1.1476 0.029 Uiso 1 1 calc R
H12B H 0.5936 0.9187 1.0547 0.029 Uiso 1 1 calc R
C13 C 0.59815(11) 0.88761(11) 1.22397(10) 0.0264(2) Uani 1 1 d .
H13A H 0.6952 0.9464 1.2441 0.032 Uiso 1 1 calc R
H13B H 0.5441 0.9069 1.2945 0.032 Uiso 1 1 calc R
C14 C 0.59990(11) 0.73374(11) 1.19190(9) 0.0246(2) Uani 1 1 d .
H14A H 0.6636 0.7169 1.1278 0.030 Uiso 1 1 calc R
H14B H 0.6360 0.7105 1.2616 0.030 Uiso 1 1 calc R
C15 C 0.45345(11) 0.63952(11) 1.15153(9) 0.0220(2) Uani 1 1 d .
H15A H 0.3921 0.6499 1.2182 0.026 Uiso 1 1 calc R
H15B H 0.4583 0.5409 1.1280 0.026 Uiso 1 1 calc R
C16 C 0.03923(10) 0.38217(10) 0.74487(9) 0.0193(2) Uani 1 1 d .
H16 H 0.1260 0.3904 0.7005 0.023 Uiso 1 1 calc R
C17 C -0.06805(13) 0.43068(11) 0.68195(10) 0.0278(2) Uani 1 1 d .
H17A H -0.0264 0.5272 0.6759 0.033 Uiso 1 1 calc R
H17B H -0.1505 0.4320 0.7297 0.033 Uiso 1 1 calc R
C18 C -0.11577(14) 0.33574(12) 0.55771(10) 0.0330(3) Uani 1 1 d .
H18A H -0.1878 0.3687 0.5217 0.040 Uiso 1 1 calc R
H18B H -0.0352 0.3410 0.5074 0.040 Uiso 1 1 calc R
C19 C -0.17587(11) 0.18480(11) 0.56221(10) 0.0265(2) Uani 1 1 d .
H19A H -0.2620 0.1779 0.6058 0.032 Uiso 1 1 calc R
H19B H -0.2013 0.1250 0.4808 0.032 Uiso 1 1 calc R
C20 C -0.07008(12) 0.13333(11) 0.62290(10) 0.0279(2) Uani 1 1 d .
H20A H 0.0109 0.1293 0.5738 0.033 Uiso 1 1 calc R
H20B H -0.1137 0.0377 0.6301 0.033 Uiso 1 1 calc R
C21 C -0.01905(11) 0.22918(10) 0.74596(10) 0.0245(2) Uani 1 1 d .
H21A H -0.0979 0.2223 0.7980 0.029 Uiso 1 1 calc R
H21B H 0.0547 0.1965 0.7797 0.029 Uiso 1 1 calc R
C22 C -0.04644(11) 0.19697(11) 1.14007(10) 0.0260(2) Uani 1 1 d .
H22A H -0.1050 0.1193 1.0780 0.031 Uiso 1 1 calc R
H22B H -0.1053 0.2581 1.1795 0.031 Uiso 1 1 calc R
C23 C 0.02083(12) 0.14191(13) 1.22860(11) 0.0305(2) Uani 1 1 d .
H23A H -0.0428 0.0568 1.2428 0.037 Uiso 1 1 calc R
H23B H 0.0478 0.2132 1.3048 0.037 Uiso 1 1 calc R
C24 C 0.14993(12) 0.10919(12) 1.16761(10) 0.0288(2) Uani 1 1 d .
H24A H 0.2297 0.1285 1.2261 0.035 Uiso 1 1 calc R
H24B H 0.1296 0.0103 1.1221 0.035 Uiso 1 1 calc R
C25 C 0.18112(13) 0.20700(13) 1.08555(11) 0.0326(3) Uani 1 1 d .
H25A H 0.2716 0.2771 1.1115 0.039 Uiso 1 1 calc R
H25B H 0.1867 0.1533 1.0036 0.039 Uiso 1 1 calc R
Li Li 0.07876(19) 0.45072(19) 1.05004(16) 0.0244(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C25 O C22 108.48(8) . .
C25 O Li 125.85(9) . .
C22 O Li 125.50(8) . .
C1 N1 C10 119.80(8) . .
C1 N1 Li 90.13(8) . .
C10 N1 Li 149.12(8) . .
C1 N2 C16 118.73(8) . .
C1 N2 Li 117.48(8) . 2_567
C16 N2 Li 115.92(8) . 2_567
C1 N2 Li 83.13(7) . .
C16 N2 Li 142.29(8) . .
Li N2 Li 71.27(8) 2_567 .
N1 C1 N2 118.89(8) . .
N1 C1 C2 120.49(9) . .
N2 C1 C2 120.58(9) . .
N1 C1 Li 56.89(7) . .
N2 C1 Li 63.58(7) . .
C2 C1 Li 168.85(8) . .
C3 C2 C1 175.39(10) . .
C2 C3 C4 178.27(11) . .
C9 C4 C5 119.23(9) . .
C9 C4 C3 119.93(9) . .
C5 C4 C3 120.84(9) . .
C6 C5 C4 119.97(10) . .
C7 C6 C5 120.38(10) . .
C6 C7 C8 120.02(10) . .
C7 C8 C9 120.15(10) . .
C8 C9 C4 120.25(10) . .
N1 C10 C15 109.76(8) . .
N1 C10 C11 111.76(8) . .
C15 C10 C11 109.74(8) . .
C12 C11 C10 111.56(8) . .
C11 C12 C13 110.87(9) . .
C14 C13 C12 111.43(9) . .
C15 C14 C13 111.06(9) . .
C14 C15 C10 111.38(8) . .
N2 C16 C17 111.89(8) . .
N2 C16 C21 108.99(8) . .
C17 C16 C21 109.82(8) . .
C16 C17 C18 112.20(9) . .
C19 C18 C17 111.06(9) . .
C20 C19 C18 110.73(9) . .
C19 C20 C21 111.50(9) . .
C16 C21 C20 113.11(9) . .
O C22 C23 104.21(9) . .
C22 C23 C24 102.73(9) . .
C25 C24 C23 103.79(9) . .
O C25 C24 107.33(9) . .
O Li N1 126.92(10) . .
O Li N2 108.03(9) . 2_567
N1 Li N2 118.44(9) . 2_567
O Li N2 122.23(9) . .
N1 Li N2 65.67(6) . .
N2 Li N2 108.73(8) 2_567 .
O Li C1 127.75(9) . .
N1 Li C1 32.98(4) . .
N2 Li C1 123.01(9) 2_567 .
N2 Li C1 33.29(4) . .
O Li Li 136.76(13) . 2_567
N1 Li Li 91.83(10) . 2_567
N2 Li Li 56.80(7) 2_567 2_567
N2 Li Li 51.93(7) . 2_567
C1 Li Li 73.40(8) . 2_567
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O C25 1.4294(13) .
O C22 1.4341(13) .
O Li 1.9518(19) .
N1 C1 1.3201(13) .
N1 C10 1.4560(12) .
N1 Li 2.031(2) .
N2 C1 1.3407(12) .
N2 C16 1.4646(12) .
N2 Li 2.0580(19) 2_567
N2 Li 2.188(2) .
C1 C2 1.4681(13) .
C1 Li 2.425(2) .
C2 C3 1.2018(14) .
C3 C4 1.4366(13) .
C4 C9 1.3979(14) .
C4 C5 1.3989(14) .
C5 C6 1.3903(15) .
C6 C7 1.3833(17) .
C7 C8 1.3869(17) .
C8 C9 1.3879(14) .
C10 C15 1.5267(14) .
C10 C11 1.5305(14) .
C11 C12 1.5294(14) .
C12 C13 1.5307(15) .
C13 C14 1.5276(15) .
C14 C15 1.5262(14) .
C16 C17 1.5289(14) .
C16 C21 1.5294(13) .
C17 C18 1.5337(15) .
C18 C19 1.5232(15) .
C19 C20 1.5219(15) .
C20 C21 1.5310(15) .
C22 C23 1.5132(15) .
C23 C24 1.5317(16) .
C24 C25 1.5269(16) .
Li N2 2.0580(19) 2_567
Li Li 2.476(4) 2_567
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C10 N1 C1 N2 -173.11(8) . .
Li N1 C1 N2 14.87(10) . .
C10 N1 C1 C2 4.79(13) . .
Li N1 C1 C2 -167.23(9) . .
C10 N1 C1 Li 172.02(11) . .
C16 N2 C1 N1 -161.31(9) . .
Li N2 C1 N1 50.81(12) 2_567 .
Li N2 C1 N1 -13.89(9) . .
C16 N2 C1 C2 20.80(13) . .
Li N2 C1 C2 -127.08(9) 2_567 .
Li N2 C1 C2 168.22(9) . .
C16 N2 C1 Li -147.42(10) . .
Li N2 C1 Li 64.70(10) 2_567 .
N1 C1 C2 C3 -41.1(13) . .
N2 C1 C2 C3 136.7(12) . .
Li C1 C2 C3 -114.3(12) . .
C1 C2 C3 C4 34(4) . .
C2 C3 C4 C9 -94(4) . .
C2 C3 C4 C5 86(4) . .
C9 C4 C5 C6 0.22(15) . .
C3 C4 C5 C6 -179.33(9) . .
C4 C5 C6 C7 0.54(16) . .
C5 C6 C7 C8 -0.79(16) . .
C6 C7 C8 C9 0.29(17) . .
C7 C8 C9 C4 0.47(16) . .
C5 C4 C9 C8 -0.72(15) . .
C3 C4 C9 C8 178.83(9) . .
C1 N1 C10 C15 -143.35(9) . .
Li N1 C10 C15 20.96(19) . .
C1 N1 C10 C11 94.65(10) . .
Li N1 C10 C11 -101.04(16) . .
N1 C10 C11 C12 179.04(8) . .
C15 C10 C11 C12 57.03(11) . .
C10 C11 C12 C13 -55.94(12) . .
C11 C12 C13 C14 54.46(12) . .
C12 C13 C14 C15 -54.84(12) . .
C13 C14 C15 C10 56.57(11) . .
N1 C10 C15 C14 179.59(8) . .
C11 C10 C15 C14 -57.21(11) . .
C1 N2 C16 C17 -118.34(10) . .
Li N2 C16 C17 30.03(11) 2_567 .
Li N2 C16 C17 122.60(12) . .
C1 N2 C16 C21 120.01(9) . .
Li N2 C16 C21 -91.63(10) 2_567 .
Li N2 C16 C21 0.94(16) . .
N2 C16 C17 C18 -175.39(9) . .
C21 C16 C17 C18 -54.22(12) . .
C16 C17 C18 C19 56.78(13) . .
C17 C18 C19 C20 -56.21(13) . .
C18 C19 C20 C21 54.86(13) . .
N2 C16 C21 C20 176.02(8) . .
C17 C16 C21 C20 53.12(12) . .
C19 C20 C21 C16 -54.27(12) . .
C25 O C22 C23 33.97(12) . .
Li O C22 C23 -141.47(10) . .
O C22 C23 C24 -36.44(11) . .
C22 C23 C24 C25 25.62(12) . .
C22 O C25 C24 -17.21(13) . .
Li O C25 C24 158.21(10) . .
C23 C24 C25 O -6.26(13) . .
C25 O Li N1 -7.59(18) . .
C22 O Li N1 167.07(10) . .
C25 O Li N2 -158.18(10) . 2_567
C22 O Li N2 16.48(15) . 2_567
C25 O Li N2 74.63(15) . .
C22 O Li N2 -110.71(12) . .
C25 O Li C1 34.24(17) . .
C22 O Li C1 -151.11(10) . .
C25 O Li Li 141.45(17) . 2_567
C22 O Li Li -43.9(2) . 2_567
C1 N1 Li O 104.40(12) . .
C10 N1 Li O -62.0(2) . .
C1 N1 Li N2 -107.67(10) . 2_567
C10 N1 Li N2 85.91(18) . 2_567
C1 N1 Li N2 -8.69(6) . .
C10 N1 Li N2 -175.12(15) . .
C10 N1 Li C1 -166.42(18) . .
C1 N1 Li Li -54.94(10) . 2_567
C10 N1 Li Li 138.63(14) . 2_567
C1 N2 Li O -111.01(11) . .
C16 N2 Li O 18.46(19) . .
Li N2 Li O 126.88(15) 2_567 .
C1 N2 Li N1 8.62(6) . .
C16 N2 Li N1 138.08(12) . .
Li N2 Li N1 -113.49(10) 2_567 .
C1 N2 Li N2 122.11(9) . 2_567
C16 N2 Li N2 -108.42(13) . 2_567
Li N2 Li N2 0.0 2_567 2_567
C16 N2 Li C1 129.46(14) . .
Li N2 Li C1 -122.11(9) 2_567 .
C1 N2 Li Li 122.11(9) . 2_567
C16 N2 Li Li -108.42(13) . 2_567
N1 C1 Li O -101.69(13) . .
N2 C1 Li O 92.84(12) . .
C2 C1 Li O -21.8(5) . .
N2 C1 Li N1 -165.47(10) . .
C2 C1 Li N1 79.9(4) . .
N1 C1 Li N2 92.42(12) . 2_567
N2 C1 Li N2 -73.05(11) . 2_567
C2 C1 Li N2 172.3(4) . 2_567
N1 C1 Li N2 165.47(10) . .
C2 C1 Li N2 -114.7(4) . .
N1 C1 Li Li 121.38(11) . 2_567
N2 C1 Li Li -44.09(8) . 2_567
C2 C1 Li Li -158.8(4) . 2_567
