#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013035.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_7013035
loop_
_publ_author_name
'Deacon, Glen B.'
'Forsyth, Craig M.'
'Scott, Natalie M.'
_publ_section_title
;
 Mixed-ligand ytterbium(iii) complexes incorporating one or two
 bidentate (N,O) amide ligands
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3216
_journal_paper_doi               10.1039/b303724j
_journal_year                    2003
_chemical_formula_sum            'C21 H25 Cl N O Si Yb'
_chemical_formula_weight         544.00
_chemical_name_common            ybcph
_chemical_name_systematic
;
Dichlorobis(methylcyclopentadienyl)bis(N-(2-phenoxyphenyl)-N-trimethy
lsilylamido)diytterbium(III)
;
_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                 98.9972(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6568(1)
_cell_length_b                   8.7267(1)
_cell_length_c                   25.3241(3)
_cell_measurement_reflns_used    20656
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      3.16
_cell_volume                     2107.85(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20656
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.630
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   empirical/multiscan
_exptl_absorpt_process_details   'SORTAV (R. Blessing 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.954
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0213
_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)+(0.0159P)²+3.8701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0511
_reflns_number_gt                4876
_reflns_number_total             5202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303724j.txt
_cod_data_source_block           compound3
_cod_original_cell_volume        2107.9(7)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7013035
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.478919(10) 0.091582(12) 0.072751(4) 0.00992(4) Uani 1 1 d . . .
Cl1 Cl 0.46816(6) -0.17459(7) 0.02261(2) 0.01460(12) Uani 1 1 d . . .
Si1 Si 0.77283(7) 0.33025(8) 0.09954(3) 0.01429(14) Uani 1 1 d . . .
O1 O 0.54299(18) -0.0719(2) 0.14669(7) 0.0142(4) Uani 1 1 d . . .
N1 N 0.6906(2) 0.1580(3) 0.11188(8) 0.0122(4) Uani 1 1 d . . .
C1 C 0.2176(3) 0.1648(3) 0.03553(11) 0.0170(5) Uani 1 1 d . . .
C2 C 0.2129(3) 0.0639(3) 0.07878(11) 0.0191(6) Uani 1 1 d . . .
H2 H 0.1740 -0.0363 0.0764 0.023 Uiso 1 1 calc R . .
C3 C 0.2757(3) 0.1373(4) 0.12636(11) 0.0206(6) Uani 1 1 d . . .
H3 H 0.2852 0.0956 0.1614 0.025 Uiso 1 1 calc R . .
C4 C 0.3218(3) 0.2826(3) 0.11265(11) 0.0204(6) Uani 1 1 d . . .
H4 H 0.3686 0.3563 0.1367 0.024 Uiso 1 1 calc R . .
C5 C 0.2859(3) 0.2996(3) 0.05649(11) 0.0180(5) Uani 1 1 d . . .
H5 H 0.3047 0.3870 0.0364 0.022 Uiso 1 1 calc R . .
C6 C 0.1571(3) 0.1360(4) -0.02214(12) 0.0249(6) Uani 1 1 d . . .
H6A H 0.1158 0.0332 -0.0257 0.037 Uiso 1 1 calc R . .
H6B H 0.2316 0.1436 -0.0442 0.037 Uiso 1 1 calc R . .
H6C H 0.0845 0.2125 -0.0340 0.037 Uiso 1 1 calc R . .
C11 C 0.7638(3) 0.0414(3) 0.14190(9) 0.0115(5) Uani 1 1 d . . .
C12 C 0.6908(3) -0.0799(3) 0.16188(10) 0.0131(5) Uani 1 1 d . . .
C13 C 0.7550(3) -0.1989(3) 0.19247(11) 0.0173(5) Uani 1 1 d . . .
H13 H 0.7005 -0.2790 0.2042 0.021 Uiso 1 1 calc R . .
C14 C 0.9001(3) -0.1999(3) 0.20574(11) 0.0206(6) Uani 1 1 d . . .
H14 H 0.9457 -0.2783 0.2280 0.025 Uiso 1 1 calc R . .
C15 C 0.9776(3) -0.0853(3) 0.18619(12) 0.0203(6) Uani 1 1 d . . .
H15 H 1.0770 -0.0865 0.1946 0.024 Uiso 1 1 calc R . .
C16 C 0.9114(3) 0.0312(3) 0.15448(10) 0.0159(5) Uani 1 1 d . . .
H16 H 0.9671 0.1067 0.1408 0.019 Uiso 1 1 calc R . .
C17 C 0.6311(3) 0.4759(3) 0.08159(12) 0.0219(6) Uani 1 1 d . . .
H17A H 0.5751 0.4837 0.1106 0.033 Uiso 1 1 calc R . .
H17B H 0.5706 0.4446 0.0486 0.033 Uiso 1 1 calc R . .
H17C H 0.6732 0.5757 0.0762 0.033 Uiso 1 1 calc R . .
C18 C 0.8772(3) 0.3192(4) 0.04346(13) 0.0251(6) Uani 1 1 d . . .
H18A H 0.8180 0.2797 0.0114 0.038 Uiso 1 1 calc R . .
H18B H 0.9573 0.2505 0.0534 0.038 Uiso 1 1 calc R . .
H18C H 0.9111 0.4217 0.0361 0.038 Uiso 1 1 calc R . .
C19 C 0.8924(3) 0.4070(3) 0.15913(13) 0.0281(7) Uani 1 1 d . . .
H19B H 0.8411 0.4150 0.1895 0.042 Uiso 1 1 calc R . .
H19A H 0.9263 0.5086 0.1507 0.042 Uiso 1 1 calc R . .
H19C H 0.9723 0.3376 0.1683 0.042 Uiso 1 1 calc R . .
C111 C 0.4579(3) -0.1620(3) 0.17540(10) 0.0146(5) Uani 1 1 d . . .
C112 C 0.4626(3) -0.1400(4) 0.22973(11) 0.0217(6) Uani 1 1 d . . .
H112 H 0.5263 -0.0687 0.2486 0.026 Uiso 1 1 calc R . .
C113 C 0.3726(3) -0.2239(4) 0.25620(11) 0.0244(6) Uani 1 1 d . . .
H113 H 0.3756 -0.2111 0.2936 0.029 Uiso 1 1 calc R . .
C114 C 0.2786(3) -0.3262(4) 0.22851(12) 0.0230(6) Uani 1 1 d . . .
H114 H 0.2164 -0.3822 0.2469 0.028 Uiso 1 1 calc R . .
C115 C 0.2749(3) -0.3473(3) 0.17400(12) 0.0201(6) Uani 1 1 d . . .
H115 H 0.2098 -0.4171 0.1550 0.024 Uiso 1 1 calc R . .
C116 C 0.3673(3) -0.2657(3) 0.14712(11) 0.0163(5) Uani 1 1 d . . .
H116 H 0.3675 -0.2813 0.1100 0.020 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Yb1 O1 72.10(7) . . ?
N1 Yb1 C4 102.47(8) . . ?
O1 Yb1 C4 100.27(8) . . ?
N1 Yb1 C3 116.73(9) . . ?
O1 Yb1 C3 78.63(8) . . ?
C4 Yb1 C3 31.67(10) . . ?
N1 Yb1 C5 118.74(8) . . ?
O1 Yb1 C5 130.07(8) . . ?
C4 Yb1 C5 31.94(8) . . ?
C3 Yb1 C5 52.32(9) . . ?
N1 Yb1 C2 148.23(8) . . ?
O1 Yb1 C2 92.07(8) . . ?
C4 Yb1 C2 52.30(9) . . ?
C3 Yb1 C2 31.60(9) . . ?
C5 Yb1 C2 51.90(9) . . ?
N1 Yb1 C1 150.12(9) . . ?
O1 Yb1 C1 123.31(8) . . ?
C4 Yb1 C1 52.42(9) . . ?
C3 Yb1 C1 52.16(9) . . ?
C5 Yb1 C1 31.37(9) . . ?
C2 Yb1 C1 31.25(9) . . ?
N1 Yb1 Cl1 114.28(6) . . ?
O1 Yb1 Cl1 80.52(5) . . ?
C4 Yb1 Cl1 141.22(7) . . ?
C3 Yb1 Cl1 114.32(7) . . ?
C5 Yb1 Cl1 124.55(6) . . ?
C2 Yb1 Cl1 88.96(7) . . ?
C1 Yb1 Cl1 94.46(6) . . ?
N1 Yb1 Cl1 92.32(6) . 3_655 ?
O1 Yb1 Cl1 145.69(5) . 3_655 ?
C4 Yb1 Cl1 113.08(7) . 3_655 ?
C3 Yb1 Cl1 135.04(7) . 3_655 ?
C5 Yb1 Cl1 84.25(7) . 3_655 ?
C2 Yb1 Cl1 114.28(7) . 3_655 ?
C1 Yb1 Cl1 85.29(7) . 3_655 ?
Cl1 Yb1 Cl1 78.51(2) . 3_655 ?
N1 Yb1 C11 24.64(7) . . ?
O1 Yb1 C11 49.97(7) . . ?
C4 Yb1 C11 113.75(8) . . ?
C3 Yb1 C11 114.25(8) . . ?
C5 Yb1 C11 138.92(8) . . ?
C2 Yb1 C11 139.52(8) . . ?
C1 Yb1 C11 165.53(7) . . ?
Cl1 Yb1 C11 96.53(5) . . ?
Cl1 Yb1 C11 106.10(5) 3_655 . ?
N1 Yb1 C12 49.86(7) . . ?
O1 Yb1 C12 24.54(6) . . ?
C4 Yb1 C12 112.42(8) . . ?
C3 Yb1 C12 99.03(8) . . ?
C5 Yb1 C12 144.28(8) . . ?
C2 Yb1 C12 116.48(8) . . ?
C1 Yb1 C12 147.64(8) . . ?
Cl1 Yb1 C12 84.25(5) . . ?
Cl1 Yb1 C12 125.66(5) 3_655 . ?
C11 Yb1 C12 26.07(7) . . ?
N1 Yb1 Si1 24.49(6) . . ?
O1 Yb1 Si1 95.86(5) . . ?
C4 Yb1 Si1 92.78(7) . . ?
C3 Yb1 Si1 117.74(7) . . ?
C5 Yb1 Si1 98.93(7) . . ?
C2 Yb1 Si1 145.07(7) . . ?
C1 Yb1 Si1 128.93(7) . . ?
Cl1 Yb1 Si1 125.89(2) . . ?
Cl1 Yb1 Si1 75.38(3) 3_655 . ?
C11 Yb1 Si1 48.97(5) . . ?
C12 Yb1 Si1 74.33(5) . . ?
Yb1 Cl1 Yb1 101.49(2) . 3_655 ?
N1 Si1 C18 113.91(13) . . ?
N1 Si1 C17 106.94(12) . . ?
C18 Si1 C17 108.15(14) . . ?
N1 Si1 C19 113.74(13) . . ?
C18 Si1 C19 107.01(15) . . ?
C17 Si1 C19 106.73(14) . . ?
N1 Si1 Yb1 31.46(7) . . ?
C18 Si1 Yb1 109.86(10) . . ?
C17 Si1 Yb1 79.45(10) . . ?
C19 Si1 Yb1 138.37(11) . . ?
C111 O1 C12 118.20(19) . . ?
C111 O1 Yb1 129.91(15) . . ?
C12 O1 Yb1 111.86(14) . . ?
C11 N1 Si1 121.21(17) . . ?
C11 N1 Yb1 114.11(16) . . ?
Si1 N1 Yb1 124.05(11) . . ?
C2 C1 C5 107.3(2) . . ?
C2 C1 C6 126.4(3) . . ?
C5 C1 C6 126.2(3) . . ?
C2 C1 Yb1 73.53(15) . . ?
C5 C1 Yb1 72.66(14) . . ?
C6 C1 Yb1 120.79(18) . . ?
C1 C2 C3 108.5(3) . . ?
C1 C2 Yb1 75.22(15) . . ?
C3 C2 Yb1 73.29(15) . . ?
C4 C3 C2 107.9(2) . . ?
C4 C3 Yb1 73.39(15) . . ?
C2 C3 Yb1 75.11(15) . . ?
C3 C4 C5 107.7(2) . . ?
C3 C4 Yb1 74.94(16) . . ?
C5 C4 Yb1 74.90(15) . . ?
C1 C5 C4 108.5(3) . . ?
C1 C5 Yb1 75.97(15) . . ?
C4 C5 Yb1 73.16(15) . . ?
N1 C11 C12 120.3(2) . . ?
N1 C11 C16 125.2(2) . . ?
C12 C11 C16 114.5(2) . . ?
N1 C11 Yb1 41.24(11) . . ?
C12 C11 Yb1 81.78(14) . . ?
C16 C11 Yb1 157.61(18) . . ?
C13 C12 C11 124.0(2) . . ?
C13 C12 O1 122.1(2) . . ?
C11 C12 O1 113.8(2) . . ?
C13 C12 Yb1 159.20(18) . . ?
C11 C12 Yb1 72.15(14) . . ?
O1 C12 Yb1 43.60(10) . . ?
C12 C13 C14 119.1(3) . . ?
C15 C14 C13 119.4(2) . . ?
C14 C15 C16 120.6(3) . . ?
C15 C16 C11 122.3(3) . . ?
C116 C111 C112 121.8(2) . . ?
C116 C111 O1 118.0(2) . . ?
C112 C111 O1 120.1(2) . . ?
C111 C112 C113 118.8(3) . . ?
C114 C113 C112 120.5(3) . . ?
C113 C114 C115 120.2(3) . . ?
C114 C115 C116 119.8(3) . . ?
C111 C116 C115 118.9(3) . . ?
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
Yb1 N1 2.205(2) . ?
Yb1 O1 2.3586(18) . ?
Yb1 C4 2.566(3) . ?
Yb1 C3 2.586(3) . ?
Yb1 C5 2.588(3) . ?
Yb1 C2 2.609(3) . ?
Yb1 C1 2.630(3) . ?
Yb1 Cl1 2.6414(7) . ?
Yb1 Cl1 2.6466(8) 3_655 ?
Yb1 C11 3.053(3) . ?
Yb1 C12 3.174(3) . ?
Yb1 Si1 3.5002(9) . ?
Cl1 Yb1 2.6466(8) 3_655 ?
Si1 N1 1.751(2) . ?
Si1 C18 1.868(3) . ?
Si1 C17 1.871(3) . ?
Si1 C19 1.875(3) . ?
O1 C111 1.417(3) . ?
O1 C12 1.420(3) . ?
N1 C11 1.395(3) . ?
C1 C2 1.411(4) . ?
C1 C5 1.412(4) . ?
C1 C6 1.507(4) . ?
C2 C3 1.414(4) . ?
C3 C4 1.406(4) . ?
C4 C5 1.418(4) . ?
C11 C12 1.409(4) . ?
C11 C16 1.414(3) . ?
C12 C13 1.383(4) . ?
C13 C14 1.389(4) . ?
C14 C15 1.386(4) . ?
C15 C16 1.388(4) . ?
C111 C116 1.379(4) . ?
C111 C112 1.383(4) . ?
C112 C113 1.387(4) . ?
C113 C114 1.383(4) . ?
C114 C115 1.388(4) . ?
C115 C116 1.399(4) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C111 O1 C12 C13 18.0(3) . . . . ?
