#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:14:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179833 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012964.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_7012964
loop_
_publ_author_name
'Christelle Gateau'
'Marinella Mazzanti'
'Jacques Pécaut'
'Frank A. Dunand'
'Lothar Helm'
_publ_section_title
;
 Solid-state and solution properties of the lanthanide complexes of a
 new nonadentate tripodal ligand derived from 1,4,7-triazacyclononane
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2428
_journal_page_last               2433
_journal_paper_doi               10.1039/b303079b
_journal_year                    2003
_chemical_formula_sum            'C27 H33 Gd N6 O9'
_chemical_formula_weight         742.84
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                 99.992(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0251(7)
_cell_length_b                   11.9508(11)
_cell_length_c                   14.9011(13)
_cell_measurement_temperature    298(2)
_cell_volume                     1407.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8207
_diffrn_reflns_theta_full        28.85
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.422
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4120
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0349
_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)+(0.0564P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                3530
_reflns_number_total             4120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303079b.txt
_cod_data_source_block           complex_Gd(tpatcn)_(3)
_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 
;
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               7012964
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, 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
Gd Gd 0.32357(4) 0.27580(3) 0.81940(3) 0.02267(10) Uani 1 1 d . . .
O11 O 0.5591(8) 0.3611(6) 0.9135(4) 0.0418(16) Uani 1 1 d . . .
O12 O 0.6782(9) 0.4298(7) 1.0496(5) 0.067(2) Uani 1 1 d . . .
O21 O 0.4693(8) 0.3190(6) 0.6986(4) 0.0433(15) Uani 1 1 d . . .
O22 O 0.5749(9) 0.4324(7) 0.6069(5) 0.061(2) Uani 1 1 d . . .
O31 O 0.4935(7) 0.1099(5) 0.8382(4) 0.0387(15) Uani 1 1 d . . .
O32 O 0.5963(7) -0.0454(5) 0.7879(5) 0.0432(16) Uani 1 1 d . . .
N1 N 0.0725(8) 0.1728(6) 0.8829(5) 0.0296(15) Uani 1 1 d . . .
N2 N 0.1034(8) 0.4171(6) 0.8783(5) 0.0317(16) Uani 1 1 d . . .
N3 N 0.0283(8) 0.2877(6) 0.7079(5) 0.0291(15) Uani 1 1 d . . .
N11 N 0.3727(8) 0.2186(6) 0.9866(5) 0.0306(15) Uani 1 1 d . . .
N21 N 0.3525(8) 0.4831(6) 0.7870(5) 0.0322(15) Uani 1 1 d . . .
N31 N 0.2640(8) 0.1309(6) 0.6909(5) 0.0286(15) Uani 1 1 d . . .
C1 C -0.0317(11) 0.2456(7) 0.9333(7) 0.038(2) Uani 1 1 d . . .
H1A H -0.0448 0.2084 0.9896 0.046 Uiso 1 1 calc R . .
H1B H -0.1434 0.2541 0.8969 0.046 Uiso 1 1 calc R . .
C2 C 0.0434(13) 0.3610(8) 0.9560(7) 0.039(2) Uani 1 1 d . . .
H2A H -0.0413 0.4079 0.9764 0.046 Uiso 1 1 calc R . .
H2B H 0.1378 0.3542 1.0061 0.046 Uiso 1 1 calc R . .
C3 C -0.0428(11) 0.4451(8) 0.8051(6) 0.038(2) Uani 1 1 d . . .
H3A H -0.0582 0.5256 0.8037 0.046 Uiso 1 1 calc R . .
H3B H -0.1442 0.4118 0.8206 0.046 Uiso 1 1 calc R . .
C4 C -0.0241(11) 0.4059(8) 0.7100(7) 0.036(2) Uani 1 1 d . . .
H4A H -0.1313 0.4156 0.6693 0.044 Uiso 1 1 calc R . .
H4B H 0.0591 0.4524 0.6878 0.044 Uiso 1 1 calc R . .
C5 C -0.1042(11) 0.2089(8) 0.7309(7) 0.039(2) Uani 1 1 d . . .
H5A H -0.1565 0.1706 0.6758 0.047 Uiso 1 1 calc R . .
H5B H -0.1914 0.2522 0.7526 0.047 Uiso 1 1 calc R . .
C6 C -0.0357(11) 0.1213(8) 0.8031(7) 0.039(2) Uani 1 1 d . . .
H6A H -0.1297 0.0831 0.8229 0.046 Uiso 1 1 calc R . .
H6B H 0.0295 0.0660 0.7764 0.046 Uiso 1 1 calc R . .
C11 C 0.1530(11) 0.0849(7) 0.9450(7) 0.038(2) Uani 1 1 d . . .
H11A H 0.2086 0.0309 0.9115 0.045 Uiso 1 1 calc R . .
H11B H 0.0683 0.0460 0.9723 0.045 Uiso 1 1 calc R . .
C12 C 0.2811(11) 0.1396(7) 1.0182(6) 0.035(2) Uani 1 1 d . . .
C13 C 0.3038(13) 0.1125(9) 1.1096(6) 0.048(2) Uani 1 1 d . . .
H13A H 0.2408 0.0555 1.1300 0.058 Uiso 1 1 calc R . .
C14 C 0.4199(14) 0.1706(11) 1.1693(7) 0.058(3) Uani 1 1 d . . .
H14A H 0.4349 0.1542 1.2312 0.069 Uiso 1 1 calc R . .
C15 C 0.5154(15) 0.2536(9) 1.1385(7) 0.052(3) Uani 1 1 d . . .
H15A H 0.5938 0.2946 1.1789 0.063 Uiso 1 1 calc R . .
C16 C 0.4909(13) 0.2745(9) 1.0443(7) 0.038(2) Uani 1 1 d . . .
C17 C 0.5845(10) 0.3628(8) 1.0006(7) 0.038(2) Uani 1 1 d . . .
C21 C 0.2031(18) 0.5157(11) 0.9097(11) 0.040(4) Uani 1 1 d . . .
H21A H 0.2812 0.4970 0.9649 0.047 Uiso 1 1 calc R . .
H21B H 0.1281 0.5737 0.9248 0.047 Uiso 1 1 calc R . .
C22 C 0.3025(13) 0.5611(8) 0.8399(6) 0.036(2) Uani 1 1 d . . .
C23 C 0.3546(15) 0.6726(8) 0.8377(7) 0.050(3) Uani 1 1 d . . .
H23A H 0.3191 0.7255 0.8761 0.060 Uiso 1 1 calc R . .
C24 C 0.4588(17) 0.7029(9) 0.7778(10) 0.068(4) Uani 1 1 d . . .
H24A H 0.4944 0.7766 0.7747 0.081 Uiso 1 1 calc R . .
C25 C 0.5101(13) 0.6215(10) 0.7220(8) 0.055(3) Uani 1 1 d . . .
H25A H 0.5815 0.6401 0.6814 0.067 Uiso 1 1 calc R . .
C26 C 0.4557(17) 0.5150(13) 0.7270(9) 0.037(4) Uani 1 1 d . . .
C27 C 0.5036(11) 0.4150(9) 0.6740(6) 0.039(2) Uani 1 1 d . . .
C31 C 0.0582(14) 0.2576(8) 0.6153(7) 0.037(2) Uani 1 1 d . . .
H31A H -0.0496 0.2526 0.5744 0.044 Uiso 1 1 calc R . .
H31B H 0.1238 0.3164 0.5929 0.044 Uiso 1 1 calc R . .
C32 C 0.1489(10) 0.1503(8) 0.6146(6) 0.034(2) Uani 1 1 d . . .
C33 C 0.1253(12) 0.0759(8) 0.5444(6) 0.040(2) Uani 1 1 d . . .
H33A H 0.0443 0.0902 0.4929 0.048 Uiso 1 1 calc R . .
C34 C 0.2209(12) -0.0205(8) 0.5491(7) 0.044(2) Uani 1 1 d . . .
H34A H 0.2042 -0.0728 0.5022 0.052 Uiso 1 1 calc R . .
C35 C 0.3438(11) -0.0372(8) 0.6267(7) 0.040(2) Uani 1 1 d . . .
H35A H 0.4136 -0.0998 0.6315 0.047 Uiso 1 1 calc R . .
C36 C 0.3597(10) 0.0401(7) 0.6955(6) 0.0309(18) Uani 1 1 d . . .
C37 C 0.4954(10) 0.0328(7) 0.7818(6) 0.0298(18) Uani 1 1 d . . .
O1 O 0.6264(14) 0.1789(11) 0.5377(10) 0.140(6) Uani 1 1 d . . .
O2 O 0.2907(12) 0.3799(7) 0.4579(6) 0.080(3) Uani 1 1 d . . .
O3 O 0.3631(10) 0.1706(8) 0.3862(5) 0.068(2) Uani 1 1 d . . .
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'
Gd Gd -0.1653 3.9035 '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
O21 Gd O11 84.7(2) . . ?
O21 Gd O31 85.6(2) . . ?
O11 Gd O31 84.7(2) . . ?
O21 Gd N21 64.5(2) . . ?
O11 Gd N21 66.7(2) . . ?
O31 Gd N21 139.5(2) . . ?
O21 Gd N11 142.1(2) . . ?
O11 Gd N11 64.3(2) . . ?
O31 Gd N11 71.0(2) . . ?
N21 Gd N11 116.3(2) . . ?
O21 Gd N31 68.4(2) . . ?
O11 Gd N31 139.1(2) . . ?
O31 Gd N31 63.7(2) . . ?
N21 Gd N31 121.9(2) . . ?
N11 Gd N31 121.7(2) . . ?
O21 Gd N3 91.0(2) . . ?
O11 Gd N3 151.5(3) . . ?
O31 Gd N3 123.1(2) . . ?
N21 Gd N3 86.0(2) . . ?
N11 Gd N3 126.7(2) . . ?
N31 Gd N3 62.5(2) . . ?
O21 Gd N1 150.7(2) . . ?
O11 Gd N1 124.1(2) . . ?
O31 Gd N1 91.5(2) . . ?
N21 Gd N1 128.0(2) . . ?
N11 Gd N1 61.8(2) . . ?
N31 Gd N1 84.2(2) . . ?
N3 Gd N1 66.4(2) . . ?
O21 Gd N2 123.3(2) . . ?
O11 Gd N2 92.2(2) . . ?
O31 Gd N2 150.6(2) . . ?
N21 Gd N2 62.5(2) . . ?
N11 Gd N2 81.3(2) . . ?
N31 Gd N2 128.2(2) . . ?
N3 Gd N2 66.8(2) . . ?
N1 Gd N2 66.2(2) . . ?
C17 O11 Gd 125.1(6) . . ?
C27 O21 Gd 125.9(6) . . ?
C37 O31 Gd 127.2(5) . . ?
C11 N1 C6 109.9(7) . . ?
C11 N1 C1 108.7(7) . . ?
C6 N1 C1 110.2(7) . . ?
C11 N1 Gd 106.0(5) . . ?
C6 N1 Gd 106.3(5) . . ?
C1 N1 Gd 115.6(5) . . ?
C21 N2 C2 110.4(9) . . ?
C21 N2 C3 111.8(9) . . ?
C2 N2 C3 110.5(7) . . ?
C21 N2 Gd 104.9(7) . . ?
C2 N2 Gd 106.8(5) . . ?
C3 N2 Gd 112.2(5) . . ?
C4 N3 C31 110.1(7) . . ?
C4 N3 C5 112.3(7) . . ?
C31 N3 C5 107.2(8) . . ?
C4 N3 Gd 105.4(5) . . ?
C31 N3 Gd 107.4(5) . . ?
C5 N3 Gd 114.5(5) . . ?
C12 N11 C16 119.9(8) . . ?
C12 N11 Gd 122.3(6) . . ?
C16 N11 Gd 117.7(6) . . ?
C22 N21 C26 118.0(9) . . ?
C22 N21 Gd 121.6(5) . . ?
C26 N21 Gd 118.7(8) . . ?
C36 N31 C32 119.2(8) . . ?
C36 N31 Gd 118.9(5) . . ?
C32 N31 Gd 121.5(6) . . ?
N1 C1 C2 113.9(7) . . ?
N2 C2 C1 113.9(8) . . ?
N2 C3 C4 114.8(7) . . ?
N3 C4 C3 112.8(8) . . ?
N3 C5 C6 113.9(7) . . ?
N1 C6 C5 111.6(7) . . ?
N1 C11 C12 108.3(7) . . ?
N11 C12 C13 121.9(9) . . ?
N11 C12 C11 113.5(8) . . ?
C13 C12 C11 124.6(9) . . ?
C14 C13 C12 118.9(10) . . ?
C13 C14 C15 120.4(9) . . ?
C14 C15 C16 118.0(10) . . ?
N11 C16 C15 120.9(10) . . ?
N11 C16 C17 114.9(8) . . ?
C15 C16 C17 124.2(9) . . ?
O12 C17 O11 125.4(10) . . ?
O12 C17 C16 119.5(9) . . ?
O11 C17 C16 115.1(8) . . ?
N2 C21 C22 113.3(11) . . ?
N21 C22 C23 122.2(10) . . ?
N21 C22 C21 113.9(8) . . ?
C23 C22 C21 123.5(10) . . ?
C24 C23 C22 119.0(12) . . ?
C23 C24 C25 118.8(10) . . ?
C26 C25 C24 119.6(12) . . ?
C25 C26 N21 122.3(13) . . ?
C25 C26 C27 126.8(12) . . ?
N21 C26 C27 110.8(11) . . ?
O21 C27 O22 122.7(10) . . ?
O21 C27 C26 118.8(9) . . ?
O22 C27 C26 118.5(10) . . ?
C32 C31 N3 112.1(7) . . ?
N31 C32 C33 121.1(8) . . ?
N31 C32 C31 114.1(8) . . ?
C33 C32 C31 124.8(8) . . ?
C32 C33 C34 120.3(9) . . ?
C33 C34 C35 117.9(8) . . ?
C36 C35 C34 119.0(8) . . ?
N31 C36 C35 122.4(8) . . ?
N31 C36 C37 114.2(7) . . ?
C35 C36 C37 123.3(8) . . ?
O32 C37 O31 126.6(8) . . ?
O32 C37 C36 117.8(8) . . ?
O31 C37 C36 115.6(7) . . ?
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
Gd O21 2.367(6) . ?
Gd O11 2.379(6) . ?
Gd O31 2.395(6) . ?
Gd N21 2.542(7) . ?
Gd N11 2.547(7) . ?
Gd N31 2.564(7) . ?
Gd N3 2.651(7) . ?
Gd N1 2.670(6) . ?
Gd N2 2.699(7) . ?
O11 C17 1.279(12) . ?
O12 C17 1.245(11) . ?
O21 C27 1.250(12) . ?
O22 C27 1.252(11) . ?
O31 C37 1.248(10) . ?
O32 C37 1.230(10) . ?
N1 C11 1.473(11) . ?
N1 C6 1.479(11) . ?
N1 C1 1.496(12) . ?
N2 C21 1.455(15) . ?
N2 C2 1.487(12) . ?
N2 C3 1.495(11) . ?
N3 C4 1.476(11) . ?
N3 C31 1.486(12) . ?
N3 C5 1.504(12) . ?
N11 C12 1.332(11) . ?
N11 C16 1.343(12) . ?
N21 C22 1.327(11) . ?
N21 C26 1.374(15) . ?
N31 C36 1.324(11) . ?
N31 C32 1.356(10) . ?
C1 C2 1.520(13) . ?
C3 C4 1.523(13) . ?
C5 C6 1.533(13) . ?
C11 C12 1.511(13) . ?
C12 C13 1.381(12) . ?
C13 C14 1.362(16) . ?
C14 C15 1.381(17) . ?
C15 C16 1.405(15) . ?
C16 C17 1.508(15) . ?
C21 C22 1.517(17) . ?
C22 C23 1.399(13) . ?
C23 C24 1.37(2) . ?
C24 C25 1.388(18) . ?
C25 C26 1.351(18) . ?
C26 C27 1.519(19) . ?
C31 C32 1.475(13) . ?
C32 C33 1.361(12) . ?
C33 C34 1.380(14) . ?
C34 C35 1.397(13) . ?
C35 C36 1.370(13) . ?
C36 C37 1.536(12) . ?
