#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:25:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180261 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/47/7114708.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_7114708
loop_
_publ_author_name
'Evans, William J.'
'Perotti, Jeremy M.'
'Doedens, Robert J.'
'Ziller, Joseph W.'
_publ_section_title
;
 The tetramethylpiperidinyl-1-oxide anion (TMPO--) as a ligand in
 lanthanide chemistry: synthesis of the per(TMPO--) complex
 [(ONC5H6Me4)2Sm( µ-ONC5H6Me4)]2
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2326
_journal_paper_doi               10.1039/b106869p
_journal_year                    2001
_chemical_formula_sum            'C38 H66 Cl2 N2 O2 Sm2'
_chemical_formula_weight         954.53
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.306(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5950(19)
_cell_length_b                   8.3464(11)
_cell_length_c                   17.584(2)
_cell_measurement_temperature    163(2)
_cell_volume                     2055.8(4)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_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      163(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20947
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        '< 1.0'
_exptl_absorpt_coefficient_mu    2.990
_exptl_absorpt_correction_T_max  0.8180
_exptl_absorpt_correction_T_min  0.5463
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+3.7826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                3567
_reflns_number_total             5015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106869p.txt
_cod_data_source_block           jp3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2055.9(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114708
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Sm1 Sm -0.109786(17) 0.39792(3) -0.450123(14) 0.01972(8) Uani 1 1 d .
Cl1 Cl 0.05320(8) 0.31157(15) -0.49454(7) 0.0270(3) Uani 1 1 d .
O1 O -0.1535(2) 0.3232(4) -0.34815(19) 0.0277(8) Uani 1 1 d .
N1 N -0.0719(3) 0.4092(5) -0.3012(2) 0.0227(8) Uani 1 1 d .
C1 C -0.1973(3) 0.2051(6) -0.5710(3) 0.0246(11) Uani 1 1 d .
C2 C -0.2444(3) 0.1808(6) -0.5118(3) 0.0246(11) Uani 1 1 d .
C3 C -0.2946(3) 0.3211(6) -0.5060(3) 0.0264(11) Uani 1 1 d .
C4 C -0.2783(4) 0.4351(6) -0.5598(3) 0.0279(12) Uani 1 1 d .
C5 C -0.2168(4) 0.3609(6) -0.6006(3) 0.0250(11) Uani 1 1 d .
C6 C -0.1427(4) 0.0812(7) -0.6029(3) 0.0401(14) Uani 1 1 d .
H6A H -0.1390 -0.0183 -0.5726 0.060 Uiso 1 1 calc R
H6B H -0.0780 0.1207 -0.5980 0.060 Uiso 1 1 calc R
H6C H -0.1754 0.0606 -0.6588 0.060 Uiso 1 1 calc R
C7 C -0.2436(4) 0.0289(6) -0.4660(3) 0.0353(13) Uani 1 1 d .
H7A H -0.2025 -0.0502 -0.4814 0.053 Uiso 1 1 calc R
H7B H -0.3087 -0.0134 -0.4774 0.053 Uiso 1 1 calc R
H7C H -0.2190 0.0511 -0.4092 0.053 Uiso 1 1 calc R
C8 C -0.3623(4) 0.3388(8) -0.4549(3) 0.0387(14) Uani 1 1 d .
H8A H -0.3889 0.4474 -0.4607 0.058 Uiso 1 1 calc R
H8B H -0.3275 0.3199 -0.3993 0.058 Uiso 1 1 calc R
H8C H -0.4142 0.2607 -0.4716 0.058 Uiso 1 1 calc R
C9 C -0.3218(4) 0.5995(7) -0.5764(4) 0.0417(14) Uani 1 1 d .
H9A H -0.2974 0.6526 -0.6165 0.063 Uiso 1 1 calc R
H9B H -0.3048 0.6629 -0.5275 0.063 Uiso 1 1 calc R
H9C H -0.3914 0.5900 -0.5960 0.063 Uiso 1 1 calc R
C10 C -0.1864(4) 0.4327(7) -0.6684(3) 0.0407(15) Uani 1 1 d .
H10A H -0.2086 0.5439 -0.6766 0.061 Uiso 1 1 calc R
H10B H -0.2142 0.3707 -0.7167 0.061 Uiso 1 1 calc R
H10C H -0.1166 0.4303 -0.6560 0.061 Uiso 1 1 calc R
C11 C -0.1074(4) 0.5556(6) -0.2670(3) 0.0285(12) Uani 1 1 d .
C12 C -0.0195(4) 0.6385(6) -0.2119(3) 0.0374(14) Uani 1 1 d .
H12A H 0.0203 0.6822 -0.2443 0.045 Uiso 1 1 calc R
H12B H -0.0410 0.7296 -0.1852 0.045 Uiso 1 1 calc R
C13 C 0.0409(4) 0.5270(7) -0.1496(3) 0.0416(15) Uani 1 1 d .
H13A H 0.0968 0.5856 -0.1164 0.050 Uiso 1 1 calc R
H13B H 0.0029 0.4872 -0.1149 0.050 Uiso 1 1 calc R
C14 C 0.0737(4) 0.3882(7) -0.1900(3) 0.0351(13) Uani 1 1 d .
H14A H 0.1121 0.3147 -0.1491 0.042 Uiso 1 1 calc R
H14B H 0.1155 0.4290 -0.2213 0.042 Uiso 1 1 calc R
C15 C -0.0086(4) 0.2946(6) -0.2446(3) 0.0265(11) Uani 1 1 d .
C16 C -0.1526(4) 0.6660(7) -0.3365(3) 0.0387(14) Uani 1 1 d .
H16A H -0.1053 0.6928 -0.3645 0.058 Uiso 1 1 calc R
H16B H -0.1746 0.7644 -0.3168 0.058 Uiso 1 1 calc R
H16C H -0.2070 0.6117 -0.3729 0.058 Uiso 1 1 calc R
C17 C -0.1818(4) 0.5161(7) -0.2239(3) 0.0408(14) Uani 1 1 d .
H17A H -0.2367 0.4637 -0.2607 0.061 Uiso 1 1 calc R
H17B H -0.2028 0.6151 -0.2039 0.061 Uiso 1 1 calc R
H17C H -0.1538 0.4440 -0.1794 0.061 Uiso 1 1 calc R
C18 C -0.0593(4) 0.1921(7) -0.1957(3) 0.0320(12) Uani 1 1 d .
H18A H -0.1121 0.1333 -0.2316 0.048 Uiso 1 1 calc R
H18B H -0.0843 0.2620 -0.1614 0.048 Uiso 1 1 calc R
H18C H -0.0138 0.1160 -0.1631 0.048 Uiso 1 1 calc R
C19 C 0.0323(4) 0.1784(7) -0.2948(3) 0.0374(13) Uani 1 1 d .
H19A H -0.0199 0.1168 -0.3299 0.056 Uiso 1 1 calc R
H19B H 0.0773 0.1049 -0.2598 0.056 Uiso 1 1 calc R
H19C H 0.0655 0.2394 -0.3267 0.056 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'
Cl Cl 0.1484 0.1585 '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
Cnt Sm1 Cl1 107.8 . .
Cnt Sm1 Cl1 107.6 3_564 .
Cnt Sm1 O1 97.5 . .
Cnt Sm1 N1 131.9 . .
O1 Sm1 N1 34.65(12) . .
O1 Sm1 C2 77.64(13) . .
N1 Sm1 C2 111.67(14) . .
O1 Sm1 C3 74.53(13) . .
N1 Sm1 C3 107.13(13) . .
C2 Sm1 C3 30.37(15) . .
O1 Sm1 C4 101.89(15) . .
N1 Sm1 C4 129.17(15) . .
C2 Sm1 C4 50.58(15) . .
C3 Sm1 C4 30.48(15) . .
O1 Sm1 C5 124.04(13) . .
N1 Sm1 C5 157.60(14) . .
C2 Sm1 C5 50.47(14) . .
C3 Sm1 C5 50.48(15) . .
C4 Sm1 C5 31.03(15) . .
O1 Sm1 C1 107.39(14) . .
N1 Sm1 C1 139.56(14) . .
C2 Sm1 C1 30.60(14) . .
C3 Sm1 C1 50.18(15) . .
C4 Sm1 C1 50.51(15) . .
C5 Sm1 C1 30.20(14) . .
O1 Sm1 Cl1 129.08(10) . .
N1 Sm1 Cl1 110.10(9) . .
C2 Sm1 Cl1 107.34(11) . .
C3 Sm1 Cl1 133.15(11) . .
C4 Sm1 Cl1 120.56(12) . .
C5 Sm1 Cl1 90.02(11) . .
C1 Sm1 Cl1 82.98(11) . .
O1 Sm1 Cl1 135.94(10) . 3_564
N1 Sm1 Cl1 109.02(10) . 3_564
C2 Sm1 Cl1 134.17(11) . 3_564
C3 Sm1 Cl1 116.22(12) . 3_564
C4 Sm1 Cl1 87.17(11) . 3_564
C5 Sm1 Cl1 84.53(10) . 3_564
C1 Sm1 Cl1 111.24(11) . 3_564
Cl1 Sm1 Cl1 76.76(4) . 3_564
Sm1 Cl1 Sm1 103.24(4) . 3_564
N1 O1 Sm1 86.7(2) . .
O1 N1 C15 108.7(4) . .
O1 N1 C11 108.1(3) . .
C15 N1 C11 117.9(4) . .
O1 N1 Sm1 58.62(18) . .
C15 N1 Sm1 125.5(3) . .
C11 N1 Sm1 116.3(3) . .
C5 C1 C2 108.5(5) . .
C5 C1 C6 124.9(5) . .
C2 C1 C6 126.3(5) . .
C5 C1 Sm1 74.9(3) . .
C2 C1 Sm1 74.0(3) . .
C6 C1 Sm1 121.4(3) . .
C3 C2 C1 107.8(4) . .
C3 C2 C7 126.3(5) . .
C1 C2 C7 125.8(5) . .
C3 C2 Sm1 75.1(3) . .
C1 C2 Sm1 75.4(3) . .
C7 C2 Sm1 117.5(3) . .
C2 C3 C4 108.9(4) . .
C2 C3 C8 124.5(5) . .
C4 C3 C8 126.4(5) . .
C2 C3 Sm1 74.5(3) . .
C4 C3 Sm1 75.0(3) . .
C8 C3 Sm1 121.0(3) . .
C3 C4 C5 106.9(4) . .
C3 C4 C9 127.2(5) . .
C5 C4 C9 125.8(5) . .
C3 C4 Sm1 74.5(3) . .
C5 C4 Sm1 74.5(3) . .
C9 C4 Sm1 119.7(3) . .
C1 C5 C4 107.8(4) . .
C1 C5 C10 126.1(5) . .
C4 C5 C10 125.9(5) . .
C1 C5 Sm1 74.9(3) . .
C4 C5 Sm1 74.4(3) . .
C10 C5 Sm1 120.9(3) . .
N1 C11 C17 113.2(4) . .
N1 C11 C16 106.7(4) . .
C17 C11 C16 108.7(4) . .
N1 C11 C12 107.1(4) . .
C17 C11 C12 111.7(4) . .
C16 C11 C12 109.2(5) . .
C13 C12 C11 113.1(4) . .
C14 C13 C12 109.2(4) . .
C13 C14 C15 113.1(4) . .
N1 C15 C14 108.7(4) . .
N1 C15 C19 106.7(4) . .
C14 C15 C19 108.7(4) . .
N1 C15 C18 114.9(4) . .
C14 C15 C18 110.5(4) . .
C19 C15 C18 107.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 Cnt 2.396 .
Sm1 O1 2.157(3) .
Sm1 N1 2.522(4) .
Sm1 C2 2.669(5) .
Sm1 C3 2.677(5) .
Sm1 C4 2.684(5) .
Sm1 C5 2.686(5) .
Sm1 C1 2.686(5) .
Sm1 Cl1 2.7985(12) .
Sm1 Cl1 2.8212(13) 3_564
Cl1 Sm1 2.8212(13) 3_564
O1 N1 1.436(5) .
N1 C15 1.498(6) .
N1 C11 1.516(6) .
C1 C5 1.399(7) .
C1 C2 1.413(7) .
C1 C6 1.508(7) .
C2 C3 1.401(7) .
C2 C7 1.500(7) .
C3 C4 1.409(7) .
C3 C8 1.517(7) .
C4 C5 1.436(7) .
C4 C9 1.505(7) .
C5 C10 1.509(7) .
C11 C17 1.524(7) .
C11 C16 1.525(7) .
C11 C12 1.537(7) .
C12 C13 1.517(8) .
C13 C14 1.506(8) .
C14 C15 1.525(7) .
C15 C19 1.540(7) .
C15 C18 1.542(7) .
