#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:34:38 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244416 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/28/7702897.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_7702897
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         'C14 H28 Lu N2 O6 3+, 3(I 1-)'
_chemical_formula_structural     '((C10 H20 O5) (H2 O) (C2 H3 N)2 Lu) (I)3'
_chemical_formula_sum            'C14 H28 I3 Lu N2 O6'
_chemical_formula_weight         876.05
_chemical_name_systematic
; 
 bis(acetonitrile)aqua(1,4,7,10,13-pentaoxacyclopentadecane)lutetium(III)
 triiodide 
;
_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             2012-12-08
_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                   18.946(7)
_cell_length_b                   11.146(4)
_cell_length_c                   11.901(5)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.7
_cell_volume                     2513.2(17)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1252
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12417
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.640
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_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    2.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.875
_refine_diff_density_min         -2.101
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0535P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                2752
_reflns_number_total             3019
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3dt51405f.txt
_cod_data_source_block           12rmjdc462x
_cod_original_cell_volume        2513.1(16)
_cod_database_code               7702897
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
Lu1 Lu 0.203745(14) 0.2500 -0.06474(2) 0.01186(12) Uani 1 2 d S
I1 I 0.20188(3) 0.2500 0.36624(4) 0.02011(14) Uani 1 2 d S
I2 I 0.94212(3) 0.2500 0.35011(4) 0.01804(14) Uani 1 2 d S
I3 I 0.48043(3) 0.2500 0.65180(4) 0.02684(16) Uani 1 2 d S
O1 O 0.1171(3) 0.2500 0.0726(4) 0.0168(10) Uani 1 2 d S
O2 O 0.16683(19) 0.0540(3) -0.0174(3) 0.0184(7) Uani 1 1 d .
O3 O 0.1708(2) 0.1385(3) -0.2190(3) 0.0276(9) Uani 1 1 d .
O4 O 0.2639(3) 0.2500 0.0990(4) 0.0205(11) Uani 1 2 d S
C1 C 0.0823(3) 0.1414(4) 0.1092(5) 0.0220(11) Uani 1 1 d .
H1A H 0.0399 0.1252 0.0629 0.026 Uiso 1 1 calc R
H1B H 0.0678 0.1477 0.1890 0.026 Uiso 1 1 calc R
C2 C 0.1363(3) 0.0444(5) 0.0942(5) 0.0224(11) Uani 1 1 d .
H2A H 0.1737 0.0526 0.1517 0.027 Uiso 1 1 calc R
H2B H 0.1139 -0.0352 0.1035 0.027 Uiso 1 1 calc R
C3 C 0.1310(3) -0.0163(4) -0.1011(5) 0.0237(12) Uani 1 1 d .
H3A H 0.0805 0.0064 -0.1049 0.028 Uiso 1 1 calc R
H3B H 0.1343 -0.1028 -0.0828 0.028 Uiso 1 1 calc R
C4 C 0.1669(3) 0.0094(4) -0.2110(5) 0.0232(12) Uani 1 1 d .
H4A H 0.2148 -0.0262 -0.2122 0.028 Uiso 1 1 calc R
H4B H 0.1394 -0.0241 -0.2743 0.028 Uiso 1 1 calc R
C5 C 0.1678(6) 0.1848(6) -0.3271(5) 0.062(3) Uani 1 1 d .
H5A H 0.1244 0.1556 -0.3646 0.075 Uiso 1 1 calc R
H5B H 0.2088 0.1556 -0.3706 0.075 Uiso 1 1 calc R
N1 N 0.3044(2) 0.1260(4) -0.1041(5) 0.0228(10) Uani 1 1 d .
C6 C 0.3583(3) 0.0812(4) -0.1064(5) 0.0211(11) Uani 1 1 d .
C7 C 0.4282(3) 0.0261(5) -0.1062(5) 0.0241(12) Uani 1 1 d .
H7A H 0.4537 0.0497 -0.1743 0.036 Uiso 1 1 calc R
H7B H 0.4233 -0.0614 -0.1044 0.036 Uiso 1 1 calc R
H7C H 0.4545 0.0529 -0.0399 0.036 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'
O O 0.0106 0.0060 '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
O4 Lu1 O3 145.59(10) . .
O4 Lu1 O3 145.59(10) . 7_565
O3 Lu1 O3 65.30(18) . 7_565
O4 Lu1 O1 75.42(18) . .
O3 Lu1 O1 111.74(15) . .
O3 Lu1 O1 111.74(15) 7_565 .
O4 Lu1 O2 86.77(10) . 7_565
O3 Lu1 O2 127.49(13) . 7_565
O3 Lu1 O2 67.09(13) 7_565 7_565
O1 Lu1 O2 67.78(9) . 7_565
O4 Lu1 O2 86.77(10) . .
O3 Lu1 O2 67.09(13) . .
O3 Lu1 O2 127.49(13) 7_565 .
O1 Lu1 O2 67.78(9) . .
O2 Lu1 O2 135.31(17) 7_565 .
O4 Lu1 N1 76.57(16) . 7_565
O3 Lu1 N1 111.74(17) . 7_565
O3 Lu1 N1 75.48(16) 7_565 7_565
O1 Lu1 N1 134.46(14) . 7_565
O2 Lu1 N1 75.48(14) 7_565 7_565
O2 Lu1 N1 144.50(13) . 7_565
O4 Lu1 N1 76.57(16) . .
O3 Lu1 N1 75.48(16) . .
O3 Lu1 N1 111.74(17) 7_565 .
O1 Lu1 N1 134.46(14) . .
O2 Lu1 N1 144.50(13) 7_565 .
O2 Lu1 N1 75.48(14) . .
N1 Lu1 N1 70.3(2) 7_565 .
C1 O1 C1 113.7(5) 7_565 .
C1 O1 Lu1 122.4(3) 7_565 .
C1 O1 Lu1 122.4(3) . .
C3 O2 C2 113.9(4) . .
C3 O2 Lu1 118.6(3) . .
C2 O2 Lu1 113.9(3) . .
C5 O3 C4 115.5(4) . .
C5 O3 Lu1 123.3(3) . .
C4 O3 Lu1 119.9(3) . .
O1 C1 C2 104.8(4) . .
O1 C1 H1A 110.8 . .
C2 C1 H1A 110.8 . .
O1 C1 H1B 110.8 . .
C2 C1 H1B 110.8 . .
H1A C1 H1B 108.9 . .
O2 C2 C1 109.1(4) . .
O2 C2 H2A 109.9 . .
C1 C2 H2A 109.9 . .
O2 C2 H2B 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
O2 C3 C4 106.6(4) . .
O2 C3 H3A 110.4 . .
C4 C3 H3A 110.4 . .
O2 C3 H3B 110.4 . .
C4 C3 H3B 110.4 . .
H3A C3 H3B 108.6 . .
O3 C4 C3 105.7(4) . .
O3 C4 H4A 110.6 . .
C3 C4 H4A 110.6 . .
O3 C4 H4B 110.6 . .
C3 C4 H4B 110.6 . .
H4A C4 H4B 108.7 . .
O3 C5 C5 111.9(3) . 7_565
O3 C5 H5A 109.2 . .
C5 C5 H5A 109.2 7_565 .
O3 C5 H5B 109.2 . .
C5 C5 H5B 109.2 7_565 .
H5A C5 H5B 107.9 . .
C6 N1 Lu1 166.0(5) . .
N1 C6 C7 178.2(6) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O4 2.257(5) .
Lu1 O3 2.303(4) .
Lu1 O3 2.303(4) 7_565
Lu1 O1 2.317(5) .
Lu1 O2 2.361(3) 7_565
Lu1 O2 2.361(3) .
Lu1 N1 2.401(4) 7_565
Lu1 N1 2.401(4) .
O1 C1 1.446(5) 7_565
O1 C1 1.446(5) .
O2 C3 1.438(6) .
O2 C2 1.453(6) .
O3 C5 1.387(7) .
O3 C4 1.444(6) .
C1 C2 1.500(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.502(8) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C5 1.453(13) 7_565
C5 H5A 0.9900 .
C5 H5B 0.9900 .
N1 C6 1.136(7) .
C6 C7 1.461(7) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O4 I1 3.391(5) .
O4 I2 3.431(5) 4_455
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_4
C1 O1 C1 C2 -163.4(3) 7_565 .
Lu1 O1 C1 C2 30.2(6) . .
C3 O2 C2 C1 -91.4(5) . .
Lu1 O2 C2 C1 48.8(5) . .
O1 C1 C2 O2 -48.7(6) . .
C2 O2 C3 C4 177.1(4) . .
Lu1 O2 C3 C4 38.9(5) . .
C5 O3 C4 C3 -148.8(7) . .
Lu1 O3 C4 C3 43.7(5) . .
O2 C3 C4 O3 -49.6(5) . .
C4 O3 C5 C5 176.6(3) . 7_565
Lu1 O3 C5 C5 -16.4(6) . 7_565
