#------------------------------------------------------------------------------
#$Date: 2016-03-23 13:46:10 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320295.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_4320295
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 N12 Sm'
_chemical_formula_weight         744.74
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_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                63.30(2)
_cell_angle_beta                 63.30(2)
_cell_angle_gamma                63.30(2)
_cell_formula_units_Z            1
_cell_length_a                   10.612(2)
_cell_length_b                   10.612(2)
_cell_length_c                   10.612(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.03
_cell_measurement_theta_min      21.63
_cell_volume                     906.8(4)
_computing_cell_refinement       'Syntex P1'
_computing_data_collection       'Syntex P1'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P1 Diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2295
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 300
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  0.9959
_exptl_absorpt_correction_T_min  0.8406
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple-black
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0046(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         -0.079
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0305P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0635
_refine_ls_wR_factor_obs         0.0628
_reflns_number_observed          1323
_reflns_number_total             1388
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010325w_01.cif
_cod_data_source_block           jtd6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' 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^)+(0.0305P)^2^+0.0000P] 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^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        906.8(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4320295
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm 0.0458(2) 0.0458(2) 0.0458(2) -0.01970(7) -0.01970(7) -0.01970(7)
N1 0.0401(11) 0.0449(12) 0.0390(11) -0.0129(9) -0.0179(9) -0.0158(10)
N2 0.0517(13) 0.0404(12) 0.0507(13) -0.0089(10) -0.0267(11) -0.0181(10)
C3 0.045(2) 0.047(2) 0.053(2) -0.0076(13) -0.0168(13) -0.0186(13)
C4 0.047(2) 0.058(2) 0.042(2) -0.0032(14) -0.0163(13) -0.0172(14)
C5 0.0367(14) 0.062(2) 0.0345(13) -0.0147(13) -0.0123(11) -0.0140(13)
C6 0.064(2) 0.089(3) 0.049(2) -0.031(2) -0.026(2) -0.018(2)
C7 0.098(3) 0.048(2) 0.097(3) -0.008(2) -0.041(3) -0.032(2)
B 0.0438(15) 0.0438(15) 0.0438(15) -0.0181(9) -0.0181(9) -0.0181(9)
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 0.0000 0.0000 0.0000 0.03901(14) Uani 1 d S .
N1 N 0.1594(2) -0.0214(2) 0.2353(2) 0.0379(5) Uani 1 d . .
N2 N 0.1449(3) -0.1167(2) 0.1911(3) 0.0436(5) Uani 1 d . .
C3 C 0.1710(3) -0.2499(3) 0.2921(3) 0.0492(7) Uani 1 d . .
C4 C 0.2031(3) -0.2426(4) 0.4015(3) 0.0526(7) Uani 1 d . .
H4 H 0.2262(3) -0.3204(4) 0.4836(3) 0.063 Uiso 1 calc R .
C5 C 0.1936(3) -0.0975(3) 0.3639(3) 0.0444(6) Uani 1 d . .
C6 C 0.2137(4) -0.0258(4) 0.4441(4) 0.0626(9) Uani 1 d G .
H6A H 0.2314(31) -0.1007(26) 0.5339(18) 0.094 Uiso 1 calc G .
H6B H 0.1264(20) 0.0544(21) 0.4681(32) 0.094 Uiso 1 calc G .
H6C H 0.2973(20) 0.0108(30) 0.3849(30) 0.094 Uiso 1 calc G .
C7 C 0.1646(5) -0.3798(4) 0.2761(5) 0.0783(11) Uani 1 d G .
H7A H 0.1055(31) -0.4318(38) 0.3676(21) 0.117 Uiso 1 calc G .
H7B H 0.2651(14) -0.4437(34) 0.2529(37) 0.117 Uiso 1 calc G .
H7C H 0.1254(36) -0.3504(39) 0.1979(26) 0.117 Uiso 1 calc G .
B B 0.1432(2) 0.1432(2) 0.1432(2) 0.0382(11) Uani 1 d S .
H1B H 0.1866(17) 0.1866(17) 0.1866(17) 0.035(12) Uiso 1 d S .
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'
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 Sm N2 75.47(7) 6 5 ?
N2 Sm N2 104.53(7) 6 . ?
N2 Sm N2 104.53(7) 5 . ?
N2 Sm N2 180.0 6 3 ?
N2 Sm N2 104.53(7) 5 3 ?
N2 Sm N2 75.47(7) . 3 ?
N2 Sm N2 75.47(7) 6 4 ?
N2 Sm N2 75.47(7) 5 4 ?
N2 Sm N2 180.0 . 4 ?
N2 Sm N2 104.53(7) 3 4 ?
N2 Sm N2 104.53(7) 6 2 ?
N2 Sm N2 180.0 5 2 ?
N2 Sm N2 75.47(7) . 2 ?
N2 Sm N2 75.47(7) 3 2 ?
N2 Sm N2 104.53(7) 4 2 ?
C5 N1 N2 109.1(2) . . ?
C5 N1 B 128.3(2) . . ?
N2 N1 B 122.6(2) . . ?
C3 N2 N1 106.9(2) . . ?
C3 N2 Sm 131.9(2) . . ?
N1 N2 Sm 117.7(2) . . ?
N2 C3 C4 109.9(3) . . ?
N2 C3 C7 120.4(3) . . ?
C4 C3 C7 129.6(3) . . ?
C5 C4 C3 106.2(3) . . ?
N1 C5 C4 107.9(2) . . ?
N1 C5 C6 122.8(3) . . ?
C4 C5 C6 129.3(3) . . ?
N1 B N1 110.92(15) . 2 ?
N1 B N1 110.92(15) . 3 ?
N1 B N1 110.92(15) 2 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
Sm N2 2.616(2) . ?
Sm N2 2.616(2) 2 ?
Sm N2 2.616(2) 5 ?
Sm N2 2.616(2) 4 ?
Sm N2 2.616(2) 3 ?
Sm N2 2.616(2) 6 ?
N1 C5 1.356(3) . ?
N1 N2 1.378(3) . ?
N1 B 1.544(3) . ?
N2 C3 1.333(4) . ?
C3 C4 1.389(4) . ?
C3 C7 1.496(4) . ?
C4 C5 1.374(4) . ?
C5 C6 1.496(4) . ?
B N1 1.544(3) 2 ?
B N1 1.544(3) 3 ?
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
C5 N1 N2 C3 -0.4(3) . . . . ?
B N1 N2 C3 177.6(2) . . . . ?
C5 N1 N2 Sm 161.0(2) . . . . ?
B N1 N2 Sm -21.1(3) . . . . ?
N2 Sm N2 C3 -53.0(3) 6 . . . ?
N2 Sm N2 C3 25.4(3) 5 . . . ?
N2 Sm N2 C3 127.0(3) 3 . . . ?
N2 Sm N2 C3 148.3(424) 4 . . . ?
N2 Sm N2 C3 -154.6(3) 2 . . . ?
N2 Sm N2 N1 151.29(14) 6 . . . ?
N2 Sm N2 N1 -130.28(14) 5 . . . ?
N2 Sm N2 N1 -28.71(14) 3 . . . ?
N2 Sm N2 N1 -7.4(460) 4 . . . ?
N2 Sm N2 N1 49.72(14) 2 . . . ?
N1 N2 C3 C4 -0.2(3) . . . . ?
Sm N2 C3 C4 -157.8(2) . . . . ?
N1 N2 C3 C7 -179.7(3) . . . . ?
Sm N2 C3 C7 22.7(5) . . . . ?
N2 C3 C4 C5 0.7(4) . . . . ?
C7 C3 C4 C5 -179.8(4) . . . . ?
N2 N1 C5 C4 0.8(3) . . . . ?
B N1 C5 C4 -177.0(2) . . . . ?
N2 N1 C5 C6 -178.6(3) . . . . ?
B N1 C5 C6 3.6(4) . . . . ?
C3 C4 C5 N1 -0.9(3) . . . . ?
C3 C4 C5 C6 178.4(3) . . . . ?
C5 N1 B N1 129.6(3) . . . 2 ?
N2 N1 B N1 -47.9(3) . . . 2 ?
C5 N1 B N1 -106.6(3) . . . 3 ?
N2 N1 B N1 75.8(2) . . . 3 ?
