#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025013.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_7025013
loop_
_publ_author_name
'Heitmann, Dennis'
'Jones, Cameron'
'Mills, David P.'
'Stasch, Andreas'
_publ_section_title
;
 Low coordinate lanthanide(II) complexes supported by bulky guanidinato
 and amidinato ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1877
_journal_page_last               1882
_journal_paper_doi               10.1039/b924367d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C70 H112 I2 N6 O2 Yb2'
_chemical_formula_weight         1669.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.374(3)
_cell_length_b                   10.524(2)
_cell_length_c                   23.481(5)
_cell_measurement_temperature    150(2)
_cell_volume                     3665.7(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_sigmaI/netI    0.1399
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10431
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.349
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0872
_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)+(0.0819P)²+19.4803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                3904
_reflns_number_total             6079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924367d.txt
_cod_data_source_block           compound9
_cod_original_cell_volume        3665.5(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7025013
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Yb1 Yb 0.62711(4) 0.60865(6) 0.52417(2) 0.0374(2) Uani 1 1 d .
I1 I 0.57355(8) 0.33108(10) 0.54232(5) 0.0559(4) Uani 1 1 d .
O1 O 0.6577(8) 0.5501(11) 0.4314(4) 0.059(3) Uani 1 1 d .
N1 N 0.6939(7) 0.6715(10) 0.6256(4) 0.031(3) Uani 1 1 d .
C1 C 0.7555(9) 0.7484(13) 0.6135(5) 0.033(3) Uani 1 1 d .
N2 N 0.7529(7) 0.7451(10) 0.5551(4) 0.027(3) Uani 1 1 d .
C2 C 0.6567(10) 0.6884(14) 0.6749(5) 0.037(4) Uani 1 1 d .
N3 N 0.8191(8) 0.8197(12) 0.6548(5) 0.043(3) Uani 1 1 d .
C3 C 0.6083(11) 0.8005(13) 0.6807(5) 0.041(4) Uani 1 1 d .
C4 C 0.5692(10) 0.8045(13) 0.7274(6) 0.040(4) Uani 1 1 d .
H4 H 0.5388 0.8800 0.7332 0.048 Uiso 1 1 calc R
C5 C 0.5718(11) 0.7063(14) 0.7654(6) 0.044(4) Uani 1 1 d .
H5 H 0.5416 0.7127 0.7958 0.053 Uiso 1 1 calc R
C6 C 0.6182(11) 0.5987(15) 0.7598(6) 0.050(4) Uani 1 1 d .
H6 H 0.6202 0.5310 0.7868 0.060 Uiso 1 1 calc R
C7 C 0.6631(11) 0.5849(13) 0.7151(6) 0.041(4) Uani 1 1 d .
C8 C 0.5996(11) 0.9091(14) 0.6379(6) 0.048(4) Uani 1 1 d .
H8 H 0.6579 0.9171 0.6268 0.057 Uiso 1 1 calc R
C9 C 0.5795(12) 1.0351(15) 0.6618(7) 0.057(5) Uani 1 1 d .
H9A H 0.5173 1.0352 0.6652 0.086 Uiso 1 1 calc R
H9B H 0.5869 1.1030 0.6349 0.086 Uiso 1 1 calc R
H9C H 0.6211 1.0491 0.7007 0.086 Uiso 1 1 calc R
C10 C 0.5273(14) 0.8832(18) 0.5832(8) 0.084(7) Uani 1 1 d .
H10A H 0.5418 0.8056 0.5645 0.127 Uiso 1 1 calc R
H10B H 0.5228 0.9548 0.5559 0.127 Uiso 1 1 calc R
H10C H 0.4697 0.8721 0.5931 0.127 Uiso 1 1 calc R
C11 C 0.7147(12) 0.4645(14) 0.7111(7) 0.051(4) Uani 1 1 d .
H11 H 0.7330 0.4656 0.6733 0.062 Uiso 1 1 calc R
C12 C 0.7977(16) 0.452(2) 0.7615(11) 0.111(8) Uani 1 1 d U
H12A H 0.7816 0.4626 0.7989 0.167 Uiso 1 1 calc R
H12B H 0.8414 0.5176 0.7581 0.167 Uiso 1 1 calc R
H12C H 0.8244 0.3679 0.7603 0.167 Uiso 1 1 calc R
C13 C 0.6591(12) 0.3474(15) 0.7123(7) 0.058(5) Uani 1 1 d .
H13A H 0.6492 0.3377 0.7516 0.086 Uiso 1 1 calc R
H13B H 0.6910 0.2727 0.7032 0.086 Uiso 1 1 calc R
H13C H 0.6009 0.3556 0.6829 0.086 Uiso 1 1 calc R
C14 C 0.8307(9) 0.7585(13) 0.5329(5) 0.033(3) Uani 1 1 d .
C15 C 0.9022(11) 0.6697(15) 0.5475(6) 0.047(4) Uani 1 1 d .
C16 C 0.9684(11) 0.6844(17) 0.5197(8) 0.058(5) Uani 1 1 d .
H16 H 1.0178 0.6270 0.5286 0.070 Uiso 1 1 calc R
C17 C 0.9669(13) 0.7809(19) 0.4785(7) 0.068(5) Uani 1 1 d .
H17 H 1.0148 0.7873 0.4601 0.082 Uiso 1 1 calc R
C18 C 0.8983(14) 0.8652(16) 0.4646(7) 0.064(5) Uani 1 1 d .
H18 H 0.8970 0.9287 0.4356 0.077 Uiso 1 1 calc R
C19 C 0.8304(11) 0.8584(15) 0.4927(7) 0.050(4) Uani 1 1 d .
C20 C 0.9002(11) 0.5641(15) 0.5902(7) 0.052(4) Uani 1 1 d .
H20 H 0.8711 0.5972 0.6207 0.063 Uiso 1 1 calc R
C21 C 0.9955(11) 0.5127(19) 0.6227(7) 0.071(6) Uani 1 1 d .
H21A H 1.0241 0.4757 0.5938 0.106 Uiso 1 1 calc R
H21B H 0.9896 0.4475 0.6512 0.106 Uiso 1 1 calc R
H21C H 1.0328 0.5827 0.6434 0.106 Uiso 1 1 calc R
C22 C 0.8450(11) 0.4515(15) 0.5594(8) 0.057(5) Uani 1 1 d .
H22A H 0.7854 0.4811 0.5370 0.086 Uiso 1 1 calc R
H22B H 0.8381 0.3893 0.5889 0.086 Uiso 1 1 calc R
H22C H 0.8760 0.4118 0.5324 0.086 Uiso 1 1 calc R
C23 C 0.7491(11) 0.9519(15) 0.4753(7) 0.053(4) Uani 1 1 d .
H23 H 0.7149 0.9484 0.5061 0.064 Uiso 1 1 calc R
C24 C 0.7833(15) 1.0864(16) 0.4722(11) 0.092(7) Uani 1 1 d .
H24A H 0.8096 1.0937 0.4385 0.137 Uiso 1 1 calc R
H24B H 0.8294 1.1060 0.5087 0.137 Uiso 1 1 calc R
H24C H 0.7331 1.1464 0.4673 0.137 Uiso 1 1 calc R
C25 C 0.6869(14) 0.913(2) 0.4162(7) 0.088(7) Uani 1 1 d .
H25A H 0.7223 0.9012 0.3874 0.132 Uiso 1 1 calc R
H25B H 0.6415 0.9791 0.4023 0.132 Uiso 1 1 calc R
H25C H 0.6568 0.8328 0.4208 0.132 Uiso 1 1 calc R
C26 C 0.8497(10) 0.7751(16) 0.7161(6) 0.046(4) Uani 1 1 d .
H26 H 0.8210 0.6899 0.7164 0.056 Uiso 1 1 calc R
C27 C 0.9495(11) 0.7519(18) 0.7371(7) 0.068(5) Uani 1 1 d .
H27A H 0.9696 0.7052 0.7068 0.102 Uiso 1 1 calc R
H27B H 0.9626 0.7018 0.7736 0.102 Uiso 1 1 calc R
H27C H 0.9812 0.8334 0.7447 0.102 Uiso 1 1 calc R
C28 C 0.8222(12) 0.853(2) 0.7637(7) 0.082(7) Uani 1 1 d .
H28A H 0.8541 0.9341 0.7690 0.123 Uiso 1 1 calc R
H28B H 0.8378 0.8054 0.8010 0.123 Uiso 1 1 calc R
H28C H 0.7570 0.8678 0.7516 0.123 Uiso 1 1 calc R
C29 C 0.8516(11) 0.9413(15) 0.6355(6) 0.052(4) Uani 1 1 d .
H29 H 0.8165 0.9540 0.5936 0.062 Uiso 1 1 calc R
C30 C 0.9511(13) 0.9427(17) 0.6352(8) 0.074(6) Uani 1 1 d .
H30A H 0.9677 0.8595 0.6224 0.111 Uiso 1 1 calc R
H30B H 0.9885 0.9610 0.6750 0.111 Uiso 1 1 calc R
H30C H 0.9608 1.0084 0.6079 0.111 Uiso 1 1 calc R
C31 C 0.8345(14) 1.0576(18) 0.6687(10) 0.087(7) Uani 1 1 d .
H31A H 0.7711 1.0591 0.6695 0.131 Uiso 1 1 calc R
H31B H 0.8480 1.1341 0.6488 0.131 Uiso 1 1 calc R
H31C H 0.8731 1.0550 0.7091 0.131 Uiso 1 1 calc R
C32 C 0.5910(13) 0.4778(19) 0.3868(7) 0.075(6) Uani 1 1 d .
H32A H 0.5524 0.5357 0.3576 0.090 Uiso 1 1 calc R
H32B H 0.5521 0.4267 0.4056 0.090 Uiso 1 1 calc R
C33 C 0.6446(13) 0.3936(19) 0.3579(8) 0.076(6) Uani 1 1 d .
H33A H 0.6227 0.4001 0.3144 0.091 Uiso 1 1 calc R
H33B H 0.6398 0.3040 0.3695 0.091 Uiso 1 1 calc R
C34 C 0.7404(14) 0.4386(18) 0.3785(8) 0.073(6) Uani 1 1 d .
H34A H 0.7773 0.3786 0.4074 0.088 Uiso 1 1 calc R
H34B H 0.7675 0.4480 0.3448 0.088 Uiso 1 1 calc R
C35 C 0.7331(11) 0.5645(18) 0.4065(7) 0.061(5) Uani 1 1 d .
H35A H 0.7888 0.5840 0.4375 0.073 Uiso 1 1 calc R
H35B H 0.7219 0.6334 0.3767 0.073 Uiso 1 1 calc R
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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_3
N2 Yb1 N1 55.4(3) .
N2 Yb1 O1 95.4(3) .
N1 Yb1 O1 145.0(4) .
N2 Yb1 I1 139.2(2) .
N1 Yb1 I1 100.5(3) .
O1 Yb1 I1 90.3(3) .
N2 Yb1 I1 130.4(2) 3_666
N1 Yb1 I1 122.8(3) 3_666
O1 Yb1 I1 90.1(3) 3_666
I1 Yb1 I1 89.82(3) 3_666
Yb1 I1 Yb1 90.18(3) 3_666
C35 O1 C32 104.6(12) .
C35 O1 Yb1 134.9(9) .
C32 O1 Yb1 120.4(9) .
C1 N1 C2 123.7(11) .
C1 N1 Yb1 95.6(7) .
C2 N1 Yb1 132.3(8) .
N1 C1 N2 111.4(10) .
N1 C1 N3 125.8(12) .
N2 C1 N3 122.7(13) .
C1 N2 C14 123.8(10) .
C1 N2 Yb1 97.5(8) .
C14 N2 Yb1 129.9(8) .
C3 C2 N1 120.8(13) .
C3 C2 C7 121.1(13) .
N1 C2 C7 117.9(12) .
C1 N3 C26 119.5(12) .
C1 N3 C29 118.7(11) .
C26 N3 C29 121.8(12) .
C4 C3 C2 116.7(13) .
C4 C3 C8 121.7(14) .
C2 C3 C8 121.6(13) .
C5 C4 C3 123.7(14) .
C4 C5 C6 119.5(15) .
C5 C6 C7 122.1(14) .
C6 C7 C2 116.9(13) .
C6 C7 C11 120.1(13) .
C2 C7 C11 123.0(13) .
C10 C8 C9 107.7(14) .
C10 C8 C3 110.7(14) .
C9 C8 C3 114.3(12) .
C12 C11 C13 106.5(15) .
C12 C11 C7 112.1(14) .
C13 C11 C7 112.1(14) .
C19 C14 C15 121.4(14) .
C19 C14 N2 117.4(13) .
C15 C14 N2 121.1(12) .
C16 C15 C14 116.2(15) .
C16 C15 C20 123.8(15) .
C14 C15 C20 120.0(14) .
C15 C16 C17 122.6(16) .
C18 C17 C16 120.9(17) .
C17 C18 C19 119.6(15) .
C18 C19 C14 119.3(14) .
C18 C19 C23 120.0(15) .
C14 C19 C23 120.4(15) .
C15 C20 C22 111.3(12) .
C15 C20 C21 113.7(14) .
C22 C20 C21 107.3(14) .
C24 C23 C25 110.5(16) .
C24 C23 C19 109.7(15) .
C25 C23 C19 109.6(14) .
N3 C26 C27 114.2(12) .
N3 C26 C28 117.9(14) .
C27 C26 C28 107.5(13) .
N3 C29 C31 115.0(14) .
N3 C29 C30 115.2(14) .
C31 C29 C30 107.8(14) .
O1 C32 C33 105.4(15) .
C32 C33 C34 106.3(15) .
C35 C34 C33 103.9(15) .
O1 C35 C34 104.3(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 N2 2.364(10) .
Yb1 N1 2.425(9) .
Yb1 O1 2.427(10) .
Yb1 I1 3.0946(14) .
Yb1 I1 3.1347(16) 3_666
I1 Yb1 3.1347(16) 3_666
O1 C35 1.436(18) .
O1 C32 1.472(18) .
N1 C1 1.332(17) .
N1 C2 1.428(16) .
C1 N2 1.364(15) .
C1 N3 1.400(16) .
N2 C14 1.432(16) .
C2 C3 1.42(2) .
C2 C7 1.429(18) .
N3 C26 1.470(16) .
N3 C29 1.487(19) .
C3 C4 1.382(19) .
C3 C8 1.505(19) .
C4 C5 1.359(18) .
C5 C6 1.36(2) .
C6 C7 1.41(2) .
C7 C11 1.51(2) .
C8 C10 1.49(2) .
C8 C9 1.503(19) .
C11 C12 1.50(3) .
C11 C13 1.50(2) .
C14 C19 1.412(19) .
C14 C15 1.42(2) .
C15 C16 1.35(2) .
C15 C20 1.50(2) .
C16 C17 1.40(2) .
C17 C18 1.35(2) .
C18 C19 1.38(2) .
C19 C23 1.56(2) .
C20 C22 1.53(2) .
C20 C21 1.56(2) .
C23 C24 1.52(2) .
C23 C25 1.52(2) .
C26 C27 1.50(2) .
C26 C28 1.53(2) .
C29 C31 1.51(2) .
C29 C30 1.53(2) .
C32 C33 1.49(2) .
C33 C34 1.50(2) .
C34 C35 1.50(2) .
