#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:34:38 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244416 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/28/7702899.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_7702899
loop_
_publ_author_name
'Champion, Martin J. D.'
'Farina, Paolo'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 Trivalent scandium, yttrium and lanthanide complexes with thia-oxa and
 selena-oxa macrocycles and crown ether coordination.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13179
_journal_page_last               13189
_journal_paper_doi               10.1039/c3dt51405f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C12 H24 I2 Lu O4 Se2 1+, I 1-, 2(C2 H3 N)'
_chemical_formula_sum            'C16 H30 I3 Lu N2 O4 Se2'
_chemical_formula_weight         1028.01
_chemical_name_systematic
; 
 diiodo(1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)lutetium(III)
 iodide acetonitrile solvate 
;
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-20
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.436(5)
_cell_length_b                   11.954(4)
_cell_length_c                   14.804(5)
_cell_measurement_reflns_used    6618
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      2.2
_cell_volume                     2731.7(16)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1535
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11879
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.989
_refine_diff_density_min         -2.543
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3265
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+45.6754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                2818
_reflns_number_total             3265
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3dt51405f.txt
_cod_data_source_block           12rmjdc42b1
_cod_original_cell_volume        2731.6(15)
_cod_database_code               7702899
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.08308(4) 0.2500 0.20887(3) 0.01816(18) Uani 1 2 d S . .
I1 I -0.03720(5) 0.06562(7) 0.15316(5) 0.0390(3) Uani 1 1 d . . .
I2 I 0.36462(8) 0.2500 0.85319(7) 0.0398(3) Uani 1 2 d S . .
Se1 Se 0.09214(10) 0.2500 0.01298(9) 0.0311(4) Uani 1 2 d S . .
Se2 Se -0.04624(11) 0.2500 0.35060(10) 0.0416(5) Uani 1 2 d S . .
O1 O 0.1947(6) 0.1264(7) 0.1632(5) 0.037(2) Uani 1 1 d D . .
O2 O 0.1254(6) 0.1298(9) 0.3263(5) 0.048(3) Uani 1 1 d D . .
C1 C 0.1760(8) 0.1300(10) 0.0014(7) 0.0367(19) Uani 0.50 1 d PD A 1
H1A H 0.1458 0.0570 0.0029 0.044 Uiso 0.50 1 calc PR A 1
H1B H 0.2064 0.1365 -0.0572 0.044 Uiso 0.50 1 calc PR A 1
C1B C 0.1760(8) 0.1300(10) 0.0014(7) 0.0367(19) Uani 0.50 1 d PD A 2
H1B1 H 0.1604 0.0843 -0.0519 0.044 Uiso 0.50 1 calc PR A 2
H1B2 H 0.2336 0.1634 -0.0103 0.044 Uiso 0.50 1 calc PR A 2
C2A C 0.2409(13) 0.136(2) 0.0774(12) 0.035(3) Uani 0.50 1 d PD A 1
H2A1 H 0.2832 0.0739 0.0717 0.041 Uiso 0.50 1 calc PR A 1
H2A2 H 0.2728 0.2074 0.0749 0.041 Uiso 0.50 1 calc PR A 1
C2B C 0.1830(16) 0.0574(16) 0.0782(10) 0.035(3) Uani 0.50 1 d PD A 2
H2B1 H 0.2331 0.0066 0.0703 0.041 Uiso 0.50 1 calc PR A 2
H2B2 H 0.1300 0.0112 0.0834 0.041 Uiso 0.50 1 calc PR A 2
C3 C 0.2212(10) 0.0408(11) 0.2236(7) 0.042(3) Uani 1 1 d . A .
H3A H 0.2825 0.0207 0.2125 0.051 Uiso 1 1 calc R . .
H3B H 0.1852 -0.0269 0.2149 0.051 Uiso 1 1 calc R . .
C4 C 0.2109(11) 0.0826(19) 0.3133(9) 0.077(7) Uani 1 1 d . A .
H4A H 0.2552 0.1407 0.3251 0.093 Uiso 1 1 calc R . .
H4B H 0.2200 0.0210 0.3571 0.093 Uiso 1 1 calc R . .
C5A C 0.0936(11) 0.118(2) 0.4141(15) 0.035(3) Uani 0.50 1 d PD A 1
H5A1 H 0.1204 0.1753 0.4530 0.041 Uiso 0.50 1 calc PR A 1
H5A2 H 0.1115 0.0435 0.4375 0.041 Uiso 0.50 1 calc PR A 1
C5B C 0.0719(13) 0.0618(16) 0.3798(13) 0.035(3) Uani 0.50 1 d PD A 2
H5B1 H 0.1070 0.0265 0.4279 0.041 Uiso 0.50 1 calc PR A 2
H5B2 H 0.0470 0.0015 0.3420 0.041 Uiso 0.50 1 calc PR A 2
C6 C 0.0013(8) 0.1267(10) 0.4211(7) 0.0367(19) Uani 0.50 1 d PD A 1
H6A H -0.0145 0.1373 0.4854 0.044 Uiso 0.50 1 calc PR A 1
H6B H -0.0253 0.0558 0.4004 0.044 Uiso 0.50 1 calc PR A 1
C6B C 0.0013(8) 0.1267(10) 0.4211(7) 0.0367(19) Uani 0.50 1 d PD A 2
H6B1 H 0.0227 0.1574 0.4791 0.044 Uiso 0.50 1 calc PR A 2
H6B2 H -0.0466 0.0745 0.4354 0.044 Uiso 0.50 1 calc PR A 2
N1 N 0.2192(18) 0.139(2) 0.5408(17) 0.060(7) Uani 0.50 1 d P . .
C7 C 0.2835(18) 0.186(3) 0.5557(16) 0.047(7) Uani 0.50 1 d P . .
C8 C 0.3681(17) 0.2500 0.5782(17) 0.080(8) Uani 1 2 d S . .
N2 N 0.1188(15) 0.1079(19) 0.6231(13) 0.042(5) Uani 0.50 1 d P . .
C9 C 0.1111(16) 0.1734(19) 0.6754(13) 0.032(5) Uani 0.50 1 d P . .
C10 C 0.1019(13) 0.2500 0.7495(12) 0.044(4) Uani 1 2 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
Lu Lu -0.4720 5.8584 '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'
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
O2 Lu1 O2 75.5(5) 7_565 .
O2 Lu1 O1 113.0(3) 7_565 .
O2 Lu1 O1 68.1(3) . .
O2 Lu1 O1 68.1(3) 7_565 7_565
O2 Lu1 O1 113.0(3) . 7_565
O1 Lu1 O1 77.2(4) . 7_565
O2 Lu1 Se2 69.8(2) 7_565 .
O2 Lu1 Se2 69.8(2) . .
O1 Lu1 Se2 135.10(17) . .
O1 Lu1 Se2 135.10(17) 7_565 .
O2 Lu1 Se1 136.6(2) 7_565 .
O2 Lu1 Se1 136.6(2) . .
O1 Lu1 Se1 71.32(18) . .
O1 Lu1 Se1 71.32(18) 7_565 .
Se2 Lu1 Se1 139.19(5) . .
O2 Lu1 I1 145.7(2) 7_565 .
O2 Lu1 I1 85.7(3) . .
O1 Lu1 I1 85.0(2) . .
O1 Lu1 I1 146.18(17) 7_565 .
Se2 Lu1 I1 76.85(3) . .
Se1 Lu1 I1 75.82(3) . .
O2 Lu1 I1 85.7(3) 7_565 7_565
O2 Lu1 I1 145.7(2) . 7_565
O1 Lu1 I1 146.18(17) . 7_565
O1 Lu1 I1 85.0(2) 7_565 7_565
Se2 Lu1 I1 76.85(3) . 7_565
Se1 Lu1 I1 75.82(3) . 7_565
I1 Lu1 I1 94.67(4) . 7_565
C1B Se1 C1 95.4(7) 7_565 .
C1 Se1 C1 95.4(7) 7_565 .
C1B Se1 Lu1 96.9(3) 7_565 .
C1 Se1 Lu1 96.9(3) 7_565 .
C1 Se1 Lu1 96.9(3) . .
C6B Se2 C6 98.2(7) 7_565 .
C6 Se2 C6 98.2(7) 7_565 .
C6B Se2 Lu1 97.4(3) 7_565 .
C6 Se2 Lu1 97.4(3) 7_565 .
C6 Se2 Lu1 97.4(3) . .
C3 O1 C2A 117.5(11) . .
C3 O1 C2B 99.5(10) . .
C2A O1 C2B 51.5(12) . .
C3 O1 Lu1 118.6(6) . .
C2A O1 Lu1 123.8(10) . .
C2B O1 Lu1 119.3(10) . .
C5A O2 C4 113.7(11) . .
C5B O2 C4 112.6(13) . .
C5A O2 Lu1 131.0(11) . .
C5B O2 Lu1 127.5(10) . .
C4 O2 Lu1 113.2(8) . .
C2A C1 Se1 110.2(11) . .
C2A C1 H1A 109.6 . .
Se1 C1 H1A 109.6 . .
C2A C1 H1B 109.6 . .
Se1 C1 H1B 109.6 . .
H1A C1 H1B 108.1 . .
O1 C2A C1 108.7(14) . .
O1 C2A H2A1 109.9 . .
C1 C2A H2A1 109.9 . .
O1 C2A H2A2 109.9 . .
C1 C2A H2A2 109.9 . .
H2A1 C2A H2A2 108.3 . .
O1 C2B H2B1 109.7 . .
O1 C2B H2B2 109.7 . .
H2B1 C2B H2B2 108.2 . .
O1 C3 C4 107.6(11) . .
O1 C3 H3A 110.2 . .
C4 C3 H3A 110.2 . .
O1 C3 H3B 110.2 . .
C4 C3 H3B 110.2 . .
H3A C3 H3B 108.5 . .
C3 C4 O2 111.1(12) . .
C3 C4 H4A 109.4 . .
O2 C4 H4A 109.4 . .
C3 C4 H4B 109.4 . .
O2 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
O2 C5A C6 114.1(15) . .
O2 C5A H5A1 108.7 . .
C6 C5A H5A1 108.7 . .
O2 C5A H5A2 108.7 . .
C6 C5A H5A2 108.7 . .
H5A1 C5A H5A2 107.6 . .
O2 C5B H5B1 109.4 . .
O2 C5B H5B2 109.4 . .
H5B1 C5B H5B2 108.0 . .
C5A C6 Se2 113.2(12) . .
C5A C6 H6A 108.9 . .
Se2 C6 H6A 108.9 . .
C5A C6 H6B 108.9 . .
Se2 C6 H6B 108.9 . .
H6A C6 H6B 107.8 . .
N1 C7 C7 119.0(19) . 7_565
N1 C7 C8 178(3) . .
C7 C7 C8 60.6(11) 7_565 .
C7 C8 C7 59(2) 7_565 .
N2 C9 C10 174(2) . .
N2 C9 C9 135.0(15) . 7_565
C10 C9 C9 50.4(10) . 7_565
C9 C10 C9 79.2(19) . 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O2 2.348(8) 7_565
Lu1 O2 2.348(8) .
Lu1 O1 2.368(8) .
Lu1 O1 2.368(8) 7_565
Lu1 Se2 2.8959(18) .
Lu1 Se1 2.9034(17) .
Lu1 I1 2.9974(10) .
Lu1 I1 2.9974(10) 7_565
Se1 C1B 1.939(12) 7_565
Se1 C1 1.939(12) 7_565
Se1 C1 1.939(12) .
Se2 C6B 1.950(12) 7_565
Se2 C6 1.950(12) 7_565
Se2 C6 1.950(12) .
O1 C3 1.420(13) .
O1 C2A 1.46(2) .
O1 C2B 1.516(15) .
O2 C5A 1.40(2) .
O2 C5B 1.404(16) .
O2 C4 1.450(16) .
C1 C2A 1.508(16) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2A H2A1 0.9900 .
C2A H2A2 0.9900 .
C2B H2B1 0.9900 .
C2B H2B2 0.9900 .
C3 C4 1.427(17) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5A C6 1.432(16) .
C5A H5A1 0.9900 .
C5A H5A2 0.9900 .
C5B H5B1 0.9900 .
C5B H5B2 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N1 C7 1.16(4) .
C7 C8 1.55(4) .
C8 C7 1.55(4) 7_565
N2 C9 1.11(3) .
C9 C10 1.44(3) .
C10 C9 1.44(3) 7_565
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
C1B Se1 C1 C2A 61.7(12) 7_565
C1 Se1 C1 C2A 61.7(12) 7_565
Lu1 Se1 C1 C2A -35.9(11) .
C3 O1 C2A C1 125.0(15) .
C2B O1 C2A C1 45.1(14) .
Lu1 O1 C2A C1 -57.7(19) .
Se1 C1 C2A O1 59.1(17) .
C2A O1 C3 C4 145.5(15) .
C2B O1 C3 C4 -163.1(15) .
Lu1 O1 C3 C4 -32.0(16) .
O1 C3 C4 O2 50(2) .
C5A O2 C4 C3 147.8(17) .
C5B O2 C4 C3 106.8(17) .
Lu1 O2 C4 C3 -46.9(19) .
C5B O2 C5A C6 -62.4(18) .
C4 O2 C5A C6 -159.3(17) .
O2 C5A C6 Se2 -44(2) .
C6B Se2 C6 C5A -68.4(13) 7_565
C6 Se2 C6 C5A -68.4(13) 7_565
Lu1 Se2 C6 C5A 30.2(12) .
