#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:50:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179818 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/14/7011483.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_7011483
loop_
_publ_author_name
'Ahrens, Birte'
'Cotton, Simon A.'
'Feeder, Neil'
'Noy, Oliver E.'
'Raithby, Paul R.'
'Teat, Simon J.'
_publ_section_title
;
 Structural variety in nitrate complexes of the heavy lanthanides with
 2,2':6',2″-terpyridine, and stereoselective replacement of
 nitrate
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2027
_journal_paper_doi               10.1039/b200480c
_journal_year                    2002
_chemical_formula_sum            'C17 H17 Lu N6 O10'
_chemical_formula_weight         640.34
_chemical_name_systematic
;
Complex 4
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.649(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7235(2)
_cell_length_b                   21.9191(3)
_cell_length_c                   11.3386(4)
_cell_measurement_reflns_used    14776
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.27
_cell_measurement_theta_min      1.80
_cell_volume                     2167.17(10)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT version 5.00 (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL PLUS (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Bruker AXS SMART'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68870
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14776
_diffrn_reflns_theta_full        29.27
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         1.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.623
_exptl_absorpt_correction_T_max  0.9132
_exptl_absorpt_correction_T_min  0.6549
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Transparent
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.232
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5825
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+3.5709P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                5138
_reflns_number_total             5825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200480c.txt
_cod_data_source_block           cam35
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011483
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.075889(15) 0.123544(6) -0.175363(12) 0.02255(7) Uani 1 1 d . . .
N1 N 0.2947(3) 0.18757(15) -0.2344(3) 0.0276(6) Uani 1 1 d . . .
C1 C 0.4214(5) 0.1625(2) -0.2801(4) 0.0349(8) Uani 1 1 d . . .
H1A H 0.4268 0.1193 -0.2872 0.042 Uiso 1 1 calc R . .
C2 C 0.5440(5) 0.1972(2) -0.3171(4) 0.0377(9) Uani 1 1 d . . .
H2A H 0.6307 0.1782 -0.3501 0.045 Uiso 1 1 calc R . .
C3 C 0.5379(4) 0.2598(2) -0.3051(4) 0.0362(9) Uani 1 1 d . . .
H3A H 0.6209 0.2845 -0.3291 0.043 Uiso 1 1 calc R . .
C4 C 0.4093(5) 0.28617(19) -0.2579(3) 0.0323(8) Uani 1 1 d . . .
H4A H 0.4036 0.3292 -0.2484 0.039 Uiso 1 1 calc R . .
C5 C 0.2878(4) 0.24905(17) -0.2241(3) 0.0262(7) Uani 1 1 d . . .
C6 C 0.1423(4) 0.27426(16) -0.1785(3) 0.0265(7) Uani 1 1 d . . .
N2 N 0.0367(3) 0.23334(13) -0.1456(3) 0.0238(6) Uani 1 1 d . . .
C7 C 0.1143(6) 0.33702(19) -0.1747(4) 0.0385(9) Uani 1 1 d . . .
H7A H 0.1909 0.3654 -0.1960 0.046 Uiso 1 1 calc R . .
C8 C -0.0277(6) 0.3568(2) -0.1393(5) 0.0472(11) Uani 1 1 d . . .
H8A H -0.0505 0.3992 -0.1385 0.057 Uiso 1 1 calc R . .
C9 C -0.1359(5) 0.3153(2) -0.1053(4) 0.0394(9) Uani 1 1 d . . .
H9A H -0.2336 0.3285 -0.0807 0.047 Uiso 1 1 calc R . .
C10 C -0.0998(4) 0.25368(17) -0.1075(3) 0.0269(7) Uani 1 1 d . . .
C11 C -0.2075(4) 0.20647(19) -0.0660(3) 0.0287(7) Uani 1 1 d . . .
N3 N -0.1602(4) 0.14786(16) -0.0743(3) 0.0294(6) Uani 1 1 d . . .
C12 C -0.3479(4) 0.2218(2) -0.0170(4) 0.0376(9) Uani 1 1 d . . .
H12A H -0.3785 0.2632 -0.0110 0.045 Uiso 1 1 calc R . .
C13 C -0.4418(5) 0.1752(3) 0.0228(4) 0.0468(12) Uani 1 1 d . . .
H13A H -0.5386 0.1845 0.0545 0.056 Uiso 1 1 calc R . .
C14 C -0.3931(6) 0.1161(3) 0.0156(5) 0.0487(12) Uani 1 1 d . . .
H14A H -0.4550 0.0839 0.0437 0.058 Uiso 1 1 calc R . .
C15 C -0.2528(5) 0.1035(2) -0.0330(4) 0.0410(9) Uani 1 1 d . . .
H15A H -0.2201 0.0623 -0.0376 0.049 Uiso 1 1 calc R . .
O1 O 0.2004(3) 0.14693(13) 0.0052(3) 0.0304(6) Uani 1 1 d . . .
N4 N 0.1563(4) 0.10054(16) 0.0645(3) 0.0352(7) Uani 1 1 d . . .
O2 O 0.0741(4) 0.06230(14) 0.0087(3) 0.0415(7) Uani 1 1 d . . .
O3 O 0.1899(5) 0.09485(18) 0.1694(3) 0.0611(11) Uani 1 1 d . . .
O4 O 0.1140(4) 0.11013(19) -0.3865(3) 0.0500(9) Uani 1 1 d . . .
N5 N -0.0064(5) 0.13857(19) -0.4168(3) 0.0413(9) Uani 1 1 d . . .
O5 O -0.0830(3) 0.16172(15) -0.3330(3) 0.0375(7) Uani 1 1 d . . .
O6 O -0.0478(6) 0.1446(2) -0.5199(3) 0.0666(13) Uani 1 1 d . . .
O7 O 0.2649(4) 0.05218(14) -0.1865(3) 0.0471(8) Uani 1 1 d . . .
N6 N 0.2820(4) -0.00142(17) -0.2265(4) 0.0429(9) Uani 1 1 d . . .
O8 O 0.1722(4) -0.03715(15) -0.2341(4) 0.0552(10) Uani 1 1 d . . .
O9 O 0.4110(5) -0.0159(2) -0.2537(7) 0.105(2) Uani 1 1 d . . .
O10 O -0.0746(3) 0.04109(13) -0.2260(3) 0.0343(6) Uani 1 1 d D . .
H10A H -0.024(6) 0.0116(16) -0.216(5) 0.051 Uiso 1 1 d D . .
C16 C -0.2262(7) 0.0314(3) -0.2913(5) 0.0559(13) Uani 1 1 d . . .
H16A H -0.2781 0.0714 -0.3009 0.067 Uiso 1 1 calc R . .
H16B H -0.2920 0.0053 -0.2426 0.067 Uiso 1 1 calc R . .
C17 C -0.2122(10) 0.0020(4) -0.4131(7) 0.090(3) Uani 1 1 d . . .
H17A H -0.3094 0.0066 -0.4578 0.136 Uiso 1 1 calc R . .
H17B H -0.1883 -0.0414 -0.4037 0.136 Uiso 1 1 calc R . .
H17C H -0.1300 0.0221 -0.4556 0.136 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'
Lu Lu -0.4720 5.8584 '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
O7 Lu1 O10 81.69(11) . . ?
O7 Lu1 O1 83.15(12) . . ?
O10 Lu1 O1 129.55(10) . . ?
O7 Lu1 O5 127.31(12) . . ?
O10 Lu1 O5 76.87(10) . . ?
O1 Lu1 O5 145.35(11) . . ?
O7 Lu1 O4 75.18(14) . . ?
O10 Lu1 O4 75.73(12) . . ?
O1 Lu1 O4 143.93(11) . . ?
O5 Lu1 O4 53.13(12) . . ?
O7 Lu1 N3 142.78(13) . . ?
O10 Lu1 N3 78.77(11) . . ?
O1 Lu1 N3 85.33(10) . . ?
O5 Lu1 N3 78.17(11) . . ?
O4 Lu1 N3 128.72(11) . . ?
O7 Lu1 N2 141.63(11) . . ?
O10 Lu1 N2 136.45(10) . . ?
O1 Lu1 N2 74.27(10) . . ?
O5 Lu1 N2 71.24(10) . . ?
O4 Lu1 N2 106.01(12) . . ?
N3 Lu1 N2 66.40(11) . . ?
O7 Lu1 N1 79.01(12) . . ?
O10 Lu1 N1 144.85(11) . . ?
O1 Lu1 N1 76.77(10) . . ?
O5 Lu1 N1 91.97(10) . . ?
O4 Lu1 N1 71.08(11) . . ?
N3 Lu1 N1 132.03(11) . . ?
N2 Lu1 N1 65.99(10) . . ?
O7 Lu1 O2 72.37(13) . . ?
O10 Lu1 O2 76.54(10) . . ?
O1 Lu1 O2 53.01(9) . . ?
O5 Lu1 O2 143.46(10) . . ?
O4 Lu1 O2 139.71(12) . . ?
N3 Lu1 O2 72.43(11) . . ?
N2 Lu1 O2 114.24(11) . . ?
N1 Lu1 O2 123.87(10) . . ?
O7 Lu1 N5 100.97(14) . . ?
O10 Lu1 N5 73.90(11) . . ?
O1 Lu1 N5 156.48(10) . . ?
O5 Lu1 N5 26.77(12) . . ?
O4 Lu1 N5 26.38(13) . . ?
N3 Lu1 N5 103.56(12) . . ?
N2 Lu1 N5 89.21(11) . . ?
N1 Lu1 N5 81.28(10) . . ?
O2 Lu1 N5 150.35(10) . . ?
O7 Lu1 N4 76.79(13) . . ?
O10 Lu1 N4 102.92(11) . . ?
O1 Lu1 N4 26.63(10) . . ?
O5 Lu1 N4 154.84(11) . . ?
O4 Lu1 N4 151.83(12) . . ?
N3 Lu1 N4 77.15(11) . . ?
N2 Lu1 N4 94.26(10) . . ?
N1 Lu1 N4 100.89(10) . . ?
O2 Lu1 N4 26.39(10) . . ?
N5 Lu1 N4 176.43(10) . . ?
C1 N1 C5 118.5(3) . . ?
C1 N1 Lu1 121.2(3) . . ?
C5 N1 Lu1 120.3(2) . . ?
N1 C1 C2 122.6(4) . . ?
C3 C2 C1 119.0(4) . . ?
C2 C3 C4 119.1(4) . . ?
C3 C4 C5 119.5(4) . . ?
N1 C5 C4 121.3(4) . . ?
N1 C5 C6 116.0(3) . . ?
C4 C5 C6 122.6(4) . . ?
N2 C6 C7 121.7(4) . . ?
N2 C6 C5 116.4(3) . . ?
C7 C6 C5 121.8(4) . . ?
C6 N2 C10 119.0(3) . . ?
C6 N2 Lu1 121.1(2) . . ?
C10 N2 Lu1 119.6(2) . . ?
C8 C7 C6 118.4(4) . . ?
C9 C8 C7 120.1(4) . . ?
C8 C9 C10 118.8(4) . . ?
N2 C10 C9 121.9(4) . . ?
N2 C10 C11 116.3(3) . . ?
C9 C10 C11 121.8(4) . . ?
N3 C11 C12 121.8(4) . . ?
N3 C11 C10 116.3(3) . . ?
C12 C11 C10 121.9(4) . . ?
C11 N3 C15 118.1(4) . . ?
C11 N3 Lu1 120.1(2) . . ?
C15 N3 Lu1 121.6(3) . . ?
C13 C12 C11 118.9(4) . . ?
C14 C13 C12 119.3(4) . . ?
C13 C14 C15 119.5(5) . . ?
N3 C15 C14 122.5(5) . . ?
N4 O1 Lu1 98.4(2) . . ?
O3 N4 O2 122.5(4) . . ?
O3 N4 O1 121.5(4) . . ?
O2 N4 O1 116.0(3) . . ?
O3 N4 Lu1 175.6(3) . . ?
O2 N4 Lu1 61.0(2) . . ?
O1 N4 Lu1 54.99(18) . . ?
N4 O2 Lu1 92.6(2) . . ?
N5 O4 Lu1 94.1(3) . . ?
O6 N5 O4 122.4(5) . . ?
O6 N5 O5 121.4(5) . . ?
O4 N5 O5 116.2(3) . . ?
O6 N5 Lu1 177.4(4) . . ?
O4 N5 Lu1 59.5(2) . . ?
O5 N5 Lu1 56.80(19) . . ?
N5 O5 Lu1 96.4(2) . . ?
N6 O7 Lu1 138.4(3) . . ?
O9 N6 O8 122.4(4) . . ?
O9 N6 O7 116.8(4) . . ?
O8 N6 O7 120.8(4) . . ?
C16 O10 Lu1 135.9(3) . . ?
O10 C16 C17 114.1(5) . . ?
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
Lu1 O7 2.279(3) . ?
Lu1 O10 2.297(3) . ?
Lu1 O1 2.346(3) . ?
Lu1 O5 2.382(3) . ?
Lu1 O4 2.444(3) . ?
Lu1 N3 2.444(3) . ?
Lu1 N2 2.455(3) . ?
Lu1 N1 2.477(3) . ?
Lu1 O2 2.482(3) . ?
Lu1 N5 2.829(4) . ?
Lu1 N4 2.834(4) . ?
N1 C1 1.351(5) . ?
N1 C5 1.354(5) . ?
C1 C2 1.387(6) . ?
C2 C3 1.381(7) . ?
C3 C4 1.383(6) . ?
C4 C5 1.398(5) . ?
C5 C6 1.491(5) . ?
C6 N2 1.346(5) . ?
C6 C7 1.398(5) . ?
N2 C10 1.354(5) . ?
C7 C8 1.383(7) . ?
C8 C9 1.374(7) . ?
C9 C10 1.387(6) . ?
C10 C11 1.484(5) . ?
C11 N3 1.353(5) . ?
C11 C12 1.400(5) . ?
N3 C15 1.355(5) . ?
C12 C13 1.391(7) . ?
C13 C14 1.368(8) . ?
C14 C15 1.384(7) . ?
O1 N4 1.284(5) . ?
N4 O3 1.224(5) . ?
N4 O2 1.261(5) . ?
O4 N5 1.260(6) . ?
N5 O6 1.222(5) . ?
N5 O5 1.282(5) . ?
O7 N6 1.270(5) . ?
N6 O9 1.218(5) . ?
N6 O8 1.238(5) . ?
O10 C16 1.512(6) . ?
C16 C17 1.532(10) . ?
