#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/24/7052463.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_7052463
loop_
_publ_author_name
'Schultz, Madeleine'
'Sofield, Chadwick D.'
'Walter, Marc D.'
'Andersen, Richard A.'
_publ_section_title
;
 Coordination complexes of bivalent ansa-ytterbocenes: synthesis,
 structure and comparison with related unbridged ytterbocenes and
 ansa-ferrocenes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              919
_journal_paper_doi               10.1039/b418550a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C46 H64 N2 Si Yb '
_chemical_formula_sum            'C46 H64 N2 Si Yb'
_chemical_formula_weight         846.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Jul 9 16:38:36 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 99.068(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8426(6)
_cell_length_b                   16.4380(9)
_cell_length_c                   22.338(1)
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    163.2
_cell_measurement_theta_max      53.0
_cell_measurement_theta_min      4.0
_cell_volume                     4294.2(4)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.052d'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      163.2
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       ω-scan
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17261
_diffrn_reflns_theta_max         23.26
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1752.00
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.20
_refine_diff_density_min         -1.42
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0000
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.0130
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0000
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                3243
_reflns_number_total             6369
_reflns_threshold_expression     I>3.00sigma
_cod_data_source_file            b418550a.txt
_cod_data_source_block           ansa-Cp#Yb(CNAr)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 52 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4294.1(3)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C46 H64 N2 Si Yb '
_cod_database_code               7052463
loop_
_symmetry_equiv_pos_as_xyz
' +x, +y, +z'
1/2-x,1/2+y,1/2-z
' -x, -y, -z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_calc_attached_atom
Yb1 0.09908(5) 0.28021(3) 0.37286(2) 0.0220 Uani 1.000 ? ?
Si1 -0.1386(3) 0.2293(3) 0.2783(2) 0.0366 Uani 1.000 ? ?
N1 0.353(1) 0.1772(7) 0.4570(5) 0.0331 Uani 1.000 ? ?
N2 0.2693(9) 0.4533(7) 0.4490(4) 0.0272 Uani 1.000 ? ?
C1 -0.096(1) 0.2005(8) 0.3602(5) 0.0286 Uani 1.000 ? ?
C2 -0.019(1) 0.1413(9) 0.3943(5) 0.0332 Uani 1.000 ? ?
C3 0.013(1) 0.1743(8) 0.4531(5) 0.0314 Uani 1.000 ? ?
C4 -0.040(1) 0.2495(7) 0.4586(5) 0.0276 Uani 1.000 ? ?
C5 -0.108(1) 0.2652(8) 0.4005(5) 0.0310 Uani 1.000 ? ?
C6 0.010(1) 0.0569(8) 0.3752(6) 0.0430 Uani 1.000 ? ?
C7 0.073(2) 0.0533(10) 0.3221(7) 0.0654 Uani 1.000 ? ?
C8 0.090(1) 0.0142(9) 0.4281(6) 0.0518 Uani 1.000 ? ?
C9 -0.102(2) 0.0071(10) 0.3635(8) 0.0967 Uani 1.000 ? ?
C10 -0.045(1) 0.2983(8) 0.5166(5) 0.0281 Uani 1.000 ? ?
C11 -0.054(1) 0.3895(8) 0.5044(5) 0.0449 Uani 1.000 ? ?
C12 0.063(1) 0.282(1) 0.5628(5) 0.0512 Uani 1.000 ? ?
C13 -0.150(1) 0.273(1) 0.5427(5) 0.0503 Uani 1.000 ? ?
C14 -0.0198(10) 0.2965(7) 0.2629(5) 0.024(3) Uani 1.000 ? ?
C15 0.020(1) 0.3787(8) 0.2767(4) 0.0278 Uani 1.000 ? ?
C16 0.139(1) 0.3816(8) 0.2791(5) 0.0312 Uani 1.000 ? ?
C17 0.181(1) 0.3038(8) 0.2666(5) 0.0275 Uani 1.000 ? ?
C18 0.085(1) 0.2523(7) 0.2557(4) 0.0236 Uani 1.000 ? ?
C19 -0.053(1) 0.4547(8) 0.2802(5) 0.0404 Uani 1.000 ? ?
C20 0.301(1) 0.283(1) 0.2574(5) 0.0401 Uani 1.000 ? ?
C21 0.317(1) 0.309(1) 0.1930(6) 0.0556 Uani 1.000 ? ?
C22 0.386(1) 0.331(1) 0.3020(6) 0.0611 Uani 1.000 ? ?
C23 0.325(1) 0.194(1) 0.2658(7) 0.0522 Uani 1.000 ? ?
C24 -0.290(1) 0.271(1) 0.2711(6) 0.0663 Uani 1.000 ? ?
C25 -0.151(1) 0.146(1) 0.2205(6) 0.0562 Uani 1.000 ? ?
C26 0.279(1) 0.2065(9) 0.4259(6) 0.0297 Uani 1.000 ? ?
C27 0.451(1) 0.1432(8) 0.4975(6) 0.0335 Uani 1.000 ? ?
C28 0.441(1) 0.1460(9) 0.5596(6) 0.0420 Uani 1.000 ? ?
C29 0.539(1) 0.1132(10) 0.5974(6) 0.0504 Uani 1.000 ? ?
C30 0.629(1) 0.082(1) 0.5743(7) 0.0548 Uani 1.000 ? ?
C31 0.632(1) 0.085(1) 0.5125(6) 0.0534 Uani 1.000 ? ?
C32 0.543(1) 0.1154(8) 0.4739(5) 0.0418 Uani 1.000 ? ?
C33 0.341(1) 0.178(1) 0.5840(6) 0.0614 Uani 1.000 ? ?
C34 0.546(1) 0.1161(10) 0.4067(6) 0.0524 Uani 1.000 ? ?
C35 0.214(1) 0.3986(8) 0.4275(5) 0.0281 Uani 1.000 ? ?
C36 0.337(1) 0.5193(8) 0.4748(5) 0.0256 Uani 1.000 ? ?
C37 0.351(1) 0.5233(9) 0.5403(6) 0.0367 Uani 1.000 ? ?
C38 0.412(1) 0.5900(10) 0.5650(6) 0.0436 Uani 1.000 ? ?
C39 0.456(1) 0.6465(8) 0.5310(7) 0.0424 Uani 1.000 ? ?
C40 0.439(1) 0.6400(9) 0.4676(7) 0.0437 Uani 1.000 ? ?
C41 0.380(1) 0.5745(8) 0.4402(6) 0.0316 Uani 1.000 ? ?
C42 0.303(1) 0.4598(9) 0.5751(5) 0.0441 Uani 1.000 ? ?
C43 0.361(1) 0.5660(9) 0.3724(6) 0.0473 Uani 1.000 ? ?
C44 -0.131(2) 0.468(2) 0.219(1) 0.026(7) Uani 0.485 ? ?
C45 0.040(3) 0.534(2) 0.279(2) 0.08(1) Uani 0.485 ? ?
C46 -0.091(3) 0.470(2) 0.337(1) 0.037(8) Uani 0.485 ? ?
C100 -0.0500 0.2061 0.4134 0.0025 Uani 0.000 ? ?
C101 0.0812 0.3226 0.2682 0.0025 Uani 0.000 ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H 0 256 0.000 0.000 'International Tables'
C 0 184 0.003 0.002 'International Tables'
Si 0 4 0.082 0.070 'International Tables'
Yb 0 4 -0.385 5.549 'International Tables'
N 0 8 0.006 0.003 'International Tables'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(26) Yb(1) C(35) 78.5(4) ? ? ? yes
C(26) Yb(1) C(100) 100.9(3) ? ? ? yes
C(26) Yb(1) C(101) 121.5(3) ? ? ? yes
C(35) Yb(1) C(100) 124.3(3) ? ? ? yes
C(35) Yb(1) C(101) 101.5(3) ? ? ? yes
C(100) Yb(1) C(101) 123.10(2) ? ? ? yes
C(1) Si(1) C(14) 103.4(5) ? ? ? yes
C(1) Si(1) C(24) 106.3(6) ? ? ? yes
C(1) Si(1) C(25) 117.7(7) ? ? ? yes
C(14) Si(1) C(24) 119.9(8) ? ? ? yes
C(14) Si(1) C(25) 106.6(6) ? ? ? yes
C(24) Si(1) C(25) 103.7(8) ? ? ? yes
C(26) N(1) C(27) 177(1) ? ? ? yes
C(35) N(2) C(36) 179(1) ? ? ? yes
C(2) C(1) C(5) 106(1) ? ? ? yes
C(1) C(2) C(3) 106(1) ? ? ? yes
C(1) C(2) C(6) 128(1) ? ? ? yes
C(3) C(2) C(6) 125(1) ? ? ? yes
C(2) C(3) C(4) 111(1) ? ? ? yes
C(3) C(4) C(5) 105(1) ? ? ? yes
C(3) C(4) C(10) 127(1) ? ? ? yes
C(5) C(4) C(10) 125(1) ? ? ? yes
C(1) C(5) C(4) 109(1) ? ? ? yes
C(2) C(6) C(7) 115(1) ? ? ? yes
C(2) C(6) C(8) 109(1) ? ? ? yes
C(2) C(6) C(9) 107(1) ? ? ? yes
C(7) C(6) C(8) 105(1) ? ? ? yes
C(7) C(6) C(9) 111(1) ? ? ? yes
C(8) C(6) C(9) 107(1) ? ? ? yes
C(4) C(10) C(11) 112.1(10) ? ? ? yes
C(4) C(10) C(12) 109(1) ? ? ? yes
C(4) C(10) C(13) 108(1) ? ? ? yes
C(11) C(10) C(12) 108(1) ? ? ? yes
C(11) C(10) C(13) 107(1) ? ? ? yes
C(12) C(10) C(13) 109(1) ? ? ? yes
C(15) C(14) C(18) 103(1) ? ? ? yes
C(14) C(15) C(16) 109(1) ? ? ? yes
C(14) C(15) C(19) 127(1) ? ? ? yes
C(16) C(15) C(19) 123(1) ? ? ? yes
C(15) C(16) C(17) 110(1) ? ? ? yes
C(16) C(17) C(18) 106(1) ? ? ? yes
C(16) C(17) C(20) 126(1) ? ? ? yes
C(18) C(17) C(20) 126(1) ? ? ? yes
C(14) C(18) C(17) 110(1) ? ? ? yes
C(17) C(20) C(21) 108(1) ? ? ? yes
C(17) C(20) C(22) 109(1) ? ? ? yes
C(17) C(20) C(23) 111(1) ? ? ? yes
C(21) C(20) C(22) 107(1) ? ? ? yes
C(21) C(20) C(23) 109(1) ? ? ? yes
C(22) C(20) C(23) 109(1) ? ? ? yes
Yb(1) C(26) N(1) 170(1) ? ? ? yes
N(1) C(27) C(28) 114(1) ? ? ? yes
N(1) C(27) C(32) 119(1) ? ? ? yes
C(28) C(27) C(32) 125(1) ? ? ? yes
C(27) C(28) C(29) 112(1) ? ? ? yes
C(27) C(28) C(33) 124(1) ? ? ? yes
C(29) C(28) C(33) 122(1) ? ? ? yes
C(28) C(29) C(30) 122(1) ? ? ? yes
C(29) C(30) C(31) 121(1) ? ? ? yes
C(30) C(31) C(32) 120(1) ? ? ? yes
C(27) C(32) C(31) 117(1) ? ? ? yes
C(27) C(32) C(34) 121(1) ? ? ? yes
C(31) C(32) C(34) 120(1) ? ? ? yes
Yb(1) C(35) N(2) 175(1) ? ? ? yes
N(2) C(36) C(37) 114(1) ? ? ? yes
N(2) C(36) C(41) 121(1) ? ? ? yes
C(37) C(36) C(41) 123(1) ? ? ? yes
C(36) C(37) C(38) 113(1) ? ? ? yes
C(36) C(37) C(42) 120(1) ? ? ? yes
C(38) C(37) C(42) 125(1) ? ? ? yes
C(37) C(38) C(39) 123(1) ? ? ? yes
C(38) C(39) C(40) 120(1) ? ? ? yes
C(39) C(40) C(41) 119(1) ? ? ? yes
C(36) C(41) C(40) 119(1) ? ? ? yes
C(36) C(41) C(43) 120(1) ? ? ? yes
C(40) C(41) C(43) 120(1) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb(1) C(1) 2.63(1) ? ? yes
Yb(1) C(2) 2.76(1) ? ? yes
Yb(1) C(4) 2.76(1) ? ? yes
Yb(1) C(5) 2.64(1) ? ? yes
Yb(1) C(14) 2.65(1) ? ? yes
Yb(1) C(15) 2.73(1) ? ? yes
Yb(1) C(16) 2.78(1) ? ? yes
Yb(1) C(17) 2.73(1) ? ? yes
Yb(1) C(18) 2.637(10) ? ? yes
Yb(1) C(26) 2.57(1) ? ? yes
Yb(1) C(35) 2.57(1) ? ? yes
Yb(1) C(100) 2.4341(6) ? ? yes
Yb(1) C(101) 2.4166(5) ? ? yes
Si(1) C(1) 1.88(1) ? ? yes
Si(1) C(14) 1.86(1) ? ? yes
Si(1) C(24) 1.90(1) ? ? yes
Si(1) C(25) 1.88(2) ? ? yes
N(1) C(26) 1.14(1) ? ? yes
N(1) C(27) 1.46(2) ? ? yes
N(2) C(35) 1.17(1) ? ? yes
N(2) C(36) 1.42(1) ? ? yes
C(1) C(2) 1.46(2) ? ? yes
C(1) C(5) 1.42(2) ? ? yes
C(2) C(3) 1.42(2) ? ? yes
C(2) C(6) 1.51(2) ? ? yes
C(3) C(4) 1.40(2) ? ? yes
C(4) C(5) 1.44(1) ? ? yes
C(4) C(10) 1.53(2) ? ? yes
C(6) C(7) 1.49(2) ? ? yes
C(6) C(8) 1.56(2) ? ? yes
C(6) C(9) 1.55(2) ? ? yes
C(10) C(11) 1.52(2) ? ? yes
C(10) C(12) 1.54(2) ? ? yes
C(10) C(13) 1.51(2) ? ? yes
C(14) C(15) 1.45(2) ? ? yes
C(14) C(18) 1.46(2) ? ? yes
C(15) C(16) 1.41(2) ? ? yes
C(15) C(19) 1.53(2) ? ? yes
C(16) C(17) 1.41(2) ? ? yes
C(17) C(18) 1.41(2) ? ? yes
C(17) C(20) 1.51(2) ? ? yes
C(19) C(44) 1.54(3) ? ? yes
C(19) C(45) 1.72(4) ? ? yes
C(19) C(46) 1.43(3) ? ? yes
C(19) C(47) 1.72(3) ? ? yes
C(19) C(48) 1.58(3) ? ? yes
C(19) C(49) 1.49(3) ? ? yes
C(20) C(21) 1.54(2) ? ? yes
C(20) C(22) 1.52(2) ? ? yes
C(20) C(23) 1.50(2) ? ? yes
C(27) C(28) 1.41(2) ? ? yes
C(27) C(32) 1.36(2) ? ? yes
C(28) C(29) 1.43(2) ? ? yes
C(28) C(33) 1.48(2) ? ? yes
C(29) C(30) 1.35(2) ? ? yes
C(30) C(31) 1.39(2) ? ? yes
C(31) C(32) 1.35(2) ? ? yes
C(32) C(34) 1.51(2) ? ? yes
C(36) C(37) 1.45(2) ? ? yes
C(36) C(41) 1.34(2) ? ? yes
C(37) C(38) 1.38(2) ? ? yes
C(37) C(42) 1.47(2) ? ? yes
C(38) C(39) 1.35(2) ? ? yes
C(39) C(40) 1.40(2) ? ? yes
C(40) C(41) 1.37(2) ? ? yes
C(41) C(43) 1.50(2) ? ? yes
