#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305275.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_4305275
loop_
_publ_author_name
'Jacqueline M. Veauthier'
'Eric J. Schelter'
'Christin N. Carlson'
'Brian L. Scott'
'Ryan E. Da Re'
'J. D. Thompson'
'Jaqueline L. Kiplinger'
'David E. Morris'
'Kevin D. John'
_publ_section_title
;
Direct Comparison of the Magnetic and Electronic Properties of Samarocene
and Ytterbocene Terpyridine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5841
_journal_page_last               5849
_journal_paper_doi               10.1021/ic8001465
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C35 H41 N3 Sm'
_chemical_formula_weight         654.06
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.540(3)
_cell_length_b                   14.011(3)
_cell_length_c                   14.152(3)
_cell_measurement_temperature    120(2)
_cell_volume                     2883.0(11)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32585
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.8861
_exptl_absorpt_correction_T_min  0.7075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0254P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                2523
_reflns_number_total             3678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8001465-file003_1.cif
_cod_data_source_block           apx302a
_cod_original_cell_volume        2883.1(10)
_cod_database_code               4305275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.5000 0.769165(13) 0.2500 0.01252(6) Uani 1 2 d S . .
N1 N 0.56215(14) 0.69367(16) 0.10337(14) 0.0186(5) Uani 1 1 d . . .
N2 N 0.5000 0.5944(2) 0.2500 0.0172(6) Uani 1 2 d S . .
C1 C 0.38470(17) 0.8392(2) 0.10902(18) 0.0219(6) Uani 1 1 d . . .
C2 C 0.38275(17) 0.91065(19) 0.17852(19) 0.0204(6) Uani 1 1 d . . .
C3 C 0.33680(16) 0.87317(19) 0.25844(16) 0.0172(5) Uani 1 1 d . . .
C4 C 0.31054(18) 0.77910(18) 0.23830(17) 0.0187(6) Uani 1 1 d . . .
C5 C 0.34112(18) 0.75695(19) 0.14615(19) 0.0205(6) Uani 1 1 d . . .
C6 C 0.4057(2) 0.8565(2) 0.00654(19) 0.0374(8) Uani 1 1 d . . .
H6A H 0.3522 0.8817 -0.0243 0.056 Uiso 1 1 calc R . .
H6B H 0.4231 0.7974 -0.0229 0.056 Uiso 1 1 calc R . .
H6C H 0.4554 0.9013 0.0013 0.056 Uiso 1 1 calc R . .
C7 C 0.4102(2) 1.01338(19) 0.1637(2) 0.0332(7) Uani 1 1 d . . .
H7A H 0.4705 1.0159 0.1362 0.050 Uiso 1 1 calc R . .
H7B H 0.4107 1.0460 0.2233 0.050 Uiso 1 1 calc R . .
H7C H 0.3670 1.0437 0.1221 0.050 Uiso 1 1 calc R . .
C8 C 0.30799(19) 0.9314(2) 0.34357(19) 0.0293(7) Uani 1 1 d . . .
H8A H 0.3587 0.9701 0.3641 0.044 Uiso 1 1 calc R . .
H8B H 0.2899 0.8893 0.3937 0.044 Uiso 1 1 calc R . .
H8C H 0.2572 0.9717 0.3268 0.044 Uiso 1 1 calc R . .
C9 C 0.24889(19) 0.7165(2) 0.2968(2) 0.0292(7) Uani 1 1 d . . .
H9A H 0.2558 0.7326 0.3624 0.044 Uiso 1 1 calc R . .
H9B H 0.2654 0.6508 0.2874 0.044 Uiso 1 1 calc R . .
H9C H 0.1861 0.7261 0.2781 0.044 Uiso 1 1 calc R . .
C10 C 0.3291(2) 0.6641(2) 0.0944(2) 0.0335(7) Uani 1 1 d . . .
H10A H 0.2814 0.6708 0.0479 0.050 Uiso 1 1 calc R . .
H10B H 0.3125 0.6150 0.1385 0.050 Uiso 1 1 calc R . .
H10C H 0.3857 0.6473 0.0637 0.050 Uiso 1 1 calc R . .
C11 C 0.59190(19) 0.7467(2) 0.03004(18) 0.0234(6) Uani 1 1 d . . .
H11 H 0.5839 0.8124 0.0332 0.028 Uiso 1 1 calc R . .
C12 C 0.63326(19) 0.7095(2) -0.04902(19) 0.0301(7) Uani 1 1 d . . .
H12 H 0.6502 0.7487 -0.0991 0.036 Uiso 1 1 calc R . .
C13 C 0.64902(19) 0.6124(2) -0.05239(19) 0.0329(8) Uani 1 1 d . . .
H13 H 0.6787 0.5853 -0.1040 0.039 Uiso 1 1 calc R . .
C14 C 0.62049(18) 0.5568(2) 0.0211(2) 0.0294(7) Uani 1 1 d . . .
H14 H 0.6318 0.4915 0.0200 0.035 Uiso 1 1 calc R . .
C15 C 0.57422(17) 0.5974(2) 0.09847(18) 0.0216(6) Uani 1 1 d . . .
C16 C 0.53840(19) 0.54236(19) 0.17667(19) 0.0209(6) Uani 1 1 d . . .
C17 C 0.5401(2) 0.4434(2) 0.1767(2) 0.0284(7) Uani 1 1 d . . .
H17 H 0.5682 0.4109 0.1272 0.034 Uiso 1 1 calc R . .
C18 C 0.5000 0.3924(3) 0.2500 0.0331(10) Uani 1 2 d S . .
H18 H 0.5000 0.3260 0.2500 0.040 Uiso 1 2 calc SR . .
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'
Sm Sm -0.1638 3.4418 '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
N2 Sm1 N1 64.95(5) . 3_655 ?
N2 Sm1 N1 64.95(5) . . ?
N1 Sm1 N1 129.90(10) 3_655 . ?
N2 Sm1 C5 86.42(6) . 3_655 ?
N1 Sm1 C5 80.40(7) 3_655 3_655 ?
N1 Sm1 C5 96.55(8) . 3_655 ?
N2 Sm1 C5 86.42(6) . . ?
N1 Sm1 C5 96.55(8) 3_655 . ?
N1 Sm1 C5 80.40(7) . . ?
C5 Sm1 C5 172.85(11) 3_655 . ?
N2 Sm1 C4 92.89(5) . 3_655 ?
N1 Sm1 C4 109.40(7) 3_655 3_655 ?
N1 Sm1 C4 73.17(7) . 3_655 ?
C5 Sm1 C4 29.72(7) 3_655 3_655 ?
C5 Sm1 C4 151.01(7) . 3_655 ?
N2 Sm1 C4 92.89(5) . . ?
N1 Sm1 C4 73.17(7) 3_655 . ?
N1 Sm1 C4 109.40(7) . . ?
C5 Sm1 C4 151.01(7) 3_655 . ?
C5 Sm1 C4 29.72(7) . . ?
C4 Sm1 C4 174.23(11) 3_655 . ?
N2 Sm1 C1 110.64(6) . 3_655 ?
N1 Sm1 C1 76.81(7) 3_655 3_655 ?
N1 Sm1 C1 121.77(7) . 3_655 ?
C5 Sm1 C1 29.68(7) 3_655 3_655 ?
C5 Sm1 C1 155.89(8) . 3_655 ?
C4 Sm1 C1 48.64(7) 3_655 3_655 ?
C4 Sm1 C1 128.71(7) . 3_655 ?
N2 Sm1 C1 110.64(6) . . ?
N1 Sm1 C1 121.77(7) 3_655 . ?
N1 Sm1 C1 76.81(7) . . ?
C5 Sm1 C1 155.89(8) 3_655 . ?
C5 Sm1 C1 29.68(7) . . ?
C4 Sm1 C1 128.71(7) 3_655 . ?
C4 Sm1 C1 48.64(7) . . ?
C1 Sm1 C1 138.73(12) 3_655 . ?
N2 Sm1 C3 121.52(6) . 3_655 ?
N1 Sm1 C3 124.40(7) 3_655 3_655 ?
N1 Sm1 C3 82.98(7) . 3_655 ?
C5 Sm1 C3 48.60(8) 3_655 3_655 ?
C5 Sm1 C3 136.60(8) . 3_655 ?
C4 Sm1 C3 29.25(8) 3_655 3_655 ?
C4 Sm1 C3 145.07(8) . 3_655 ?
C1 Sm1 C3 48.23(7) 3_655 3_655 ?
C1 Sm1 C3 107.31(8) . 3_655 ?
N2 Sm1 C3 121.52(6) . . ?
N1 Sm1 C3 82.98(7) 3_655 . ?
N1 Sm1 C3 124.40(7) . . ?
C5 Sm1 C3 136.60(8) 3_655 . ?
C5 Sm1 C3 48.60(8) . . ?
C4 Sm1 C3 145.07(8) 3_655 . ?
C4 Sm1 C3 29.25(8) . . ?
C1 Sm1 C3 107.31(8) 3_655 . ?
C1 Sm1 C3 48.23(7) . . ?
C3 Sm1 C3 116.96(11) 3_655 . ?
N2 Sm1 C2 135.00(6) . 3_655 ?
N1 Sm1 C2 102.69(7) 3_655 3_655 ?
N1 Sm1 C2 112.28(7) . 3_655 ?
C5 Sm1 C2 48.60(8) 3_655 3_655 ?
C5 Sm1 C2 138.55(8) . 3_655 ?
C4 Sm1 C2 48.44(7) 3_655 3_655 ?
C4 Sm1 C2 126.31(8) . 3_655 ?
C1 Sm1 C2 29.09(7) 3_655 3_655 ?
C1 Sm1 C2 112.05(8) . 3_655 ?
C3 Sm1 C2 29.32(7) 3_655 3_655 ?
C3 Sm1 C2 97.62(7) . 3_655 ?
C11 N1 C15 117.7(2) . . ?
C11 N1 Sm1 121.51(18) . . ?
C15 N1 Sm1 120.54(17) . . ?
C16 N2 C16 116.5(3) 3_655 . ?
C16 N2 Sm1 121.75(16) 3_655 . ?
C16 N2 Sm1 121.75(16) . . ?
C2 C1 C5 108.1(2) . . ?
C2 C1 C6 124.5(3) . . ?
C5 C1 C6 125.5(3) . . ?
C2 C1 Sm1 76.20(15) . . ?
C5 C1 Sm1 73.55(14) . . ?
C6 C1 Sm1 128.76(17) . . ?
C1 C2 C3 107.8(2) . . ?
C1 C2 C7 125.3(2) . . ?
C3 C2 C7 126.2(3) . . ?
C1 C2 Sm1 74.71(15) . . ?
C3 C2 Sm1 74.70(14) . . ?
C7 C2 Sm1 124.32(18) . . ?
C4 C3 C2 108.4(2) . . ?
C4 C3 C8 126.4(2) . . ?
C2 C3 C8 124.5(2) . . ?
C4 C3 Sm1 74.43(15) . . ?
C2 C3 Sm1 75.98(14) . . ?
C8 C3 Sm1 123.46(16) . . ?
C3 C4 C5 108.0(2) . . ?
C3 C4 C9 126.8(2) . . ?
C5 C4 C9 124.6(2) . . ?
C3 C4 Sm1 76.32(15) . . ?
C5 C4 Sm1 74.36(15) . . ?
C9 C4 Sm1 122.15(18) . . ?
C4 C5 C1 107.7(2) . . ?
C4 C5 C10 127.1(3) . . ?
C1 C5 C10 125.1(2) . . ?
C4 C5 Sm1 75.92(15) . . ?
C1 C5 Sm1 76.77(15) . . ?
C10 C5 Sm1 114.41(17) . . ?
N1 C11 C12 124.0(3) . . ?
C11 C12 C13 118.4(3) . . ?
C14 C13 C12 119.1(3) . . ?
C13 C14 C15 120.6(3) . . ?
N1 C15 C14 120.1(3) . . ?
N1 C15 C16 116.3(2) . . ?
C14 C15 C16 123.6(3) . . ?
N2 C16 C17 122.2(3) . . ?
N2 C16 C15 116.0(2) . . ?
C17 C16 C15 121.8(3) . . ?
C16 C17 C18 120.5(3) . . ?
C17 C18 C17 118.1(4) 3_655 . ?
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
Sm1 N2 2.449(3) . ?
Sm1 N1 2.498(2) 3_655 ?
Sm1 N1 2.498(2) . ?
Sm1 C5 2.743(3) 3_655 ?
Sm1 C5 2.743(3) . ?
Sm1 C4 2.763(3) 3_655 ?
Sm1 C4 2.763(3) . ?
Sm1 C1 2.785(3) 3_655 ?
Sm1 C1 2.785(3) . ?
Sm1 C3 2.787(2) 3_655 ?
Sm1 C3 2.787(2) . ?
Sm1 C2 2.804(3) 3_655 ?
N1 C11 1.347(3) . ?
N1 C15 1.363(3) . ?
N2 C16 1.386(3) 3_655 ?
N2 C16 1.386(3) . ?
C1 C2 1.404(4) . ?
C1 C5 1.416(4) . ?
C1 C6 1.502(3) . ?
C2 C3 1.415(3) . ?
C2 C7 1.508(4) . ?
C3 C4 1.401(4) . ?
C3 C8 1.514(3) . ?
C4 C5 1.412(3) . ?
C4 C9 1.503(4) . ?
C5 C10 1.503(4) . ?
C11 C12 1.373(4) . ?
C12 C13 1.380(4) . ?
C13 C14 1.364(4) . ?
C14 C15 1.405(4) . ?
C15 C16 1.446(4) . ?
C16 C17 1.387(4) . ?
C17 C18 1.388(4) . ?
C18 C17 1.388(4) 3_655 ?
