#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:47:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179306 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320303.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_4320303
loop_
_publ_author_name
'Anna C. Hillier'
'XingWang Zhang'
'Graham H. Maunder'
'Sung Ying Liu'
'Todd A. Eberspacher'
'Mathew V. Metz'
'Robert McDonald'
'Ângela Domingos'
'Noémia Marques'
'Victor W. Day'
'Andrea Sella'
'Josef Takats'
_publ_contact_author_address
; Department of Chemistry
   University of Alberta
   Edmonton Alberta T6G 2G2
   Canada
;
_publ_contact_author_email       joe.takats@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr Josef Takats'
_publ_contact_author_phone       1(780)4924944
_publ_section_title
;
 Synthesis and Structural Comparison of a Series of Divalent Ln(TpR,R')2
 (Ln = Sm, Eu, Yb) and Trivalent Sm(TpMe2)2X (X = F, Cl, I, BPh4)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5106
_journal_page_last               5116
_journal_paper_doi               10.1021/ic010325w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H44 B2 I N12 Sm'
_chemical_formula_weight         871.64
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5150(10)
_cell_length_b                   13.050(2)
_cell_length_c                   8.4900(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1828.9(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1744
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.488
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             866
_refine_diff_density_max         1.860
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.451
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0630P)²+5.1596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1394
_refine_ls_wR_factor_obs         0.0983
_reflns_number_observed          1502
_reflns_number_total             1689
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010325w_09.cif
_cod_data_source_block           sml2ib
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+5.1596P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+5.1596P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320303
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Sm Sm 0.5000 0.0000 0.5000 0.0308(2) Uani 1 d S .
I I 0.0000 0.0000 0.0000 0.0895(4) Uani 1 d S .
N11 N 0.3434(2) 0.0973(3) 0.6885(4) 0.0317(9) Uani 1 d . .
N12 N 0.4244(2) 0.1146(3) 0.6669(5) 0.0371(10) Uani 1 d . .
N21 N 0.2965(3) 0.0000 0.4445(6) 0.0309(12) Uani 1 d S .
N22 N 0.3664(3) 0.0000 0.3613(7) 0.0359(13) Uani 1 d S .
C13 C 0.4417(3) 0.2067(5) 0.7290(7) 0.0451(13) Uani 1 d . .
C14 C 0.3733(3) 0.2481(5) 0.7909(7) 0.0491(14) Uani 1 d . .
H14 H 0.3691(3) 0.3107(5) 0.8426(7) 0.050(16) Uiso 1 calc R .
C15 C 0.3127(3) 0.1795(5) 0.7616(6) 0.0426(13) Uani 1 d . .
C16 C 0.2243(4) 0.1874(6) 0.7988(9) 0.073(2) Uani 1 d . .
H16A H 0.1966(4) 0.1265(6) 0.7635(9) 0.160(18) Uiso 1 calc R .
H16B H 0.2010(4) 0.2460(6) 0.7460(9) 0.160(18) Uiso 1 calc R .
H16C H 0.2190(4) 0.1948(6) 0.9105(9) 0.160(18) Uiso 1 calc R .
C17 C 0.5258(4) 0.2493(6) 0.7260(9) 0.072(2) Uani 1 d . .
H17A H 0.5604(4) 0.2017(6) 0.6739(9) 0.160(18) Uiso 1 calc R .
H17B H 0.5460(4) 0.2601(6) 0.8320(9) 0.160(18) Uiso 1 calc R .
H17C H 0.5251(4) 0.3133(6) 0.6702(9) 0.160(18) Uiso 1 calc R .
C23 C 0.3418(5) 0.0000 0.2090(9) 0.042(2) Uani 1 d S .
C24 C 0.2591(5) 0.0000 0.1962(10) 0.049(2) Uani 1 d S .
H24 H 0.2277(5) 0.0000 0.1034(10) 0.099(41) Uiso 1 calc SR .
C25 C 0.2313(4) 0.0000 0.3465(9) 0.039(2) Uani 1 d S .
C26 C 0.1463(4) 0.0000 0.4035(11) 0.060(2) Uani 1 d S .
H26A H 0.1474(4) 0.0000 0.5166(11) 0.188(32) Uiso 1 calc SR .
H26B H 0.1185(4) -0.0601 0.3652(11) 0.188(32) Uiso 0.50 calc PR .
H26C H 0.1185(4) 0.0601 0.3652(11) 0.188(32) Uiso 0.50 calc PR .
C27 C 0.4043(6) 0.0000 0.0817(9) 0.065(3) Uani 1 d S .
H27A H 0.4577(6) 0.0000 0.1297(9) 0.188(32) Uiso 1 calc SR .
H27B H 0.3974(6) 0.0601 0.0174(9) 0.188(32) Uiso 0.50 calc PR .
H27C H 0.3974(6) -0.0601 0.0174(9) 0.188(32) Uiso 0.50 calc PR .
B1 B 0.3002(4) 0.0000 0.6277(9) 0.030(2) Uani 1 d S .
H1B H 0.2448(4) 0.0000 0.6656(9) 0.036 Uiso 1 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'
B B 0.0013 0.0007 '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'
I I -0.4742 1.8119 '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
N12 Sm N12 75.9(2) 5_656 2_656 ?
N12 Sm N12 180.0 5_656 . ?
N12 Sm N12 104.1(2) 2_656 . ?
N12 Sm N12 104.1(2) 5_656 6 ?
N12 Sm N12 180.0 2_656 6 ?
N12 Sm N12 75.9(2) . 6 ?
N12 Sm N22 100.92(13) 5_656 . ?
N12 Sm N22 100.92(13) 2_656 . ?
N12 Sm N22 79.08(13) . . ?
N12 Sm N22 79.08(13) 6 . ?
N12 Sm N22 79.08(13) 5_656 5_656 ?
N12 Sm N22 79.08(13) 2_656 5_656 ?
N12 Sm N22 100.92(13) . 5_656 ?
N12 Sm N22 100.92(13) 6 5_656 ?
N22 Sm N22 180.0 . 5_656 ?
N11 B1 N11 111.3(5) . 6 ?
N11 B1 N21 109.8(3) . . ?
N11 B1 N21 109.8(3) 6 . ?
C15 N11 N12 108.2(4) . . ?
C15 N11 B1 129.4(4) . . ?
N12 N11 B1 122.3(4) . . ?
C13 N12 N11 106.9(4) . . ?
C13 N12 Sm 132.4(3) . . ?
N11 N12 Sm 119.7(3) . . ?
N12 C13 C14 109.7(5) . . ?
N12 C13 C17 120.8(5) . . ?
C14 C13 C17 129.5(6) . . ?
C15 C14 C13 106.3(5) . . ?
N11 C15 C14 108.9(4) . . ?
N11 C15 C16 122.2(5) . . ?
C14 C15 C16 128.9(5) . . ?
C25 N21 N22 110.7(5) . . ?
C25 N21 B1 128.9(5) . . ?
N22 N21 B1 120.4(5) . . ?
C23 N22 N21 105.1(5) . . ?
C23 N22 Sm 134.3(4) . . ?
N21 N22 Sm 120.6(4) . . ?
N22 C23 C24 110.4(6) . . ?
N22 C23 C27 119.6(7) . . ?
C24 C23 C27 130.1(7) . . ?
C23 C24 C25 106.8(7) . . ?
N21 C25 C24 107.0(6) . . ?
N21 C25 C26 122.8(7) . . ?
C24 C25 C26 130.1(7) . . ?
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
Sm N12 2.431(4) 5_656 ?
Sm N12 2.431(4) 2_656 ?
Sm N12 2.431(4) . ?
Sm N12 2.431(4) 6 ?
Sm N22 2.469(6) . ?
Sm N22 2.469(6) 5_656 ?
B1 N11 1.537(6) . ?
B1 N11 1.537(6) 6 ?
B1 N21 1.555(9) . ?
N11 C15 1.347(6) . ?
N11 N12 1.375(5) . ?
N12 C13 1.340(7) . ?
C13 C14 1.372(7) . ?
C13 C17 1.498(7) . ?
C14 C15 1.360(8) . ?
C15 C16 1.507(7) . ?
N21 C25 1.340(9) . ?
N21 N22 1.372(7) . ?
N22 C23 1.343(10) . ?
C23 C24 1.367(11) . ?
C23 C27 1.518(10) . ?
C24 C25 1.369(12) . ?
C25 C26 1.500(10) . ?
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
N11 B1 N11 C15 -128.7(5) 6 . . . ?
N21 B1 N11 C15 109.4(6) . . . . ?
N11 B1 N11 N12 54.5(7) 6 . . . ?
N21 B1 N11 N12 -67.4(6) . . . . ?
C15 N11 N12 C13 0.7(6) . . . . ?
B1 N11 N12 C13 178.1(5) . . . . ?
C15 N11 N12 Sm -169.6(3) . . . . ?
B1 N11 N12 Sm 7.8(6) . . . . ?
N12 Sm N12 C13 -140.8(1000) 5_656 . . . ?
N12 Sm N12 C13 -34.1(5) 2_656 . . . ?
N12 Sm N12 C13 145.9(5) 6 . . . ?
N22 Sm N12 C13 -132.7(5) . . . . ?
N22 Sm N12 C13 47.3(5) 5_656 . . . ?
N12 Sm N12 N11 26.6(1000) 5_656 . . . ?
N12 Sm N12 N11 133.3(4) 2_656 . . . ?
N12 Sm N12 N11 -46.7(4) 6 . . . ?
N22 Sm N12 N11 34.7(3) . . . . ?
N22 Sm N12 N11 -145.3(3) 5_656 . . . ?
N11 N12 C13 C14 0.4(6) . . . . ?
Sm N12 C13 C14 169.0(4) . . . . ?
N11 N12 C13 C17 179.7(6) . . . . ?
Sm N12 C13 C17 -11.7(9) . . . . ?
N12 C13 C14 C15 -1.4(7) . . . . ?
C17 C13 C14 C15 179.4(7) . . . . ?
N12 N11 C15 C14 -1.6(6) . . . . ?
B1 N11 C15 C14 -178.7(5) . . . . ?
N12 N11 C15 C16 178.0(6) . . . . ?
B1 N11 C15 C16 0.8(9) . . . . ?
C13 C14 C15 N11 1.8(7) . . . . ?
C13 C14 C15 C16 -177.7(7) . . . . ?
N11 B1 N21 C25 -118.6(4) . . . . ?
N11 B1 N21 C25 118.6(4) 6 . . . ?
N11 B1 N21 N22 61.4(4) . . . . ?
N11 B1 N21 N22 -61.4(4) 6 . . . ?
C25 N21 N22 C23 0.0 . . . . ?
B1 N21 N22 C23 180.0 . . . . ?
C25 N21 N22 Sm 180.0 . . . . ?
B1 N21 N22 Sm 0.0 . . . . ?
N12 Sm N22 C23 -38.80(10) 5_656 . . . ?
N12 Sm N22 C23 38.80(10) 2_656 . . . ?
N12 Sm N22 C23 141.20(10) . . . . ?
N12 Sm N22 C23 -141.20(10) 6 . . . ?
N22 Sm N22 C23 180.0(1000) 5_656 . . . ?
N12 Sm N22 N21 141.20(10) 5_656 . . . ?
N12 Sm N22 N21 -141.20(10) 2_656 . . . ?
N12 Sm N22 N21 -38.80(10) . . . . ?
N12 Sm N22 N21 38.80(10) 6 . . . ?
N22 Sm N22 N21 0.0(1000) 5_656 . . . ?
N21 N22 C23 C24 0.0 . . . . ?
Sm N22 C23 C24 180.0 . . . . ?
N21 N22 C23 C27 180.0 . . . . ?
Sm N22 C23 C27 0.0 . . . . ?
N22 C23 C24 C25 0.0 . . . . ?
C27 C23 C24 C25 180.0 . . . . ?
N22 N21 C25 C24 0.0 . . . . ?
B1 N21 C25 C24 180.0 . . . . ?
N22 N21 C25 C26 180.0 . . . . ?
B1 N21 C25 C26 0.000(1) . . . . ?
C23 C24 C25 N21 0.0 . . . . ?
C23 C24 C25 C26 180.0 . . . . ?
