#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/50/7035003.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_7035003
loop_
_publ_author_name
'Anastasiadis, Nikolaos C.'
'Kalofolias, Dimitris A.'
'Philippidis, Aggelos'
'Tzani, Sofia'
'Raptopoulou, Catherine P.'
'Psycharis, Vassilis'
'Milios, Constantinos J.'
'Escuer, Albert'
'Perlepes, Spyros P.'
_publ_section_title
;
 A family of dinuclear lanthanide(iii) complexes from the use of a
 tridentate Schiff base.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10200
_journal_page_last               10209
_journal_paper_doi               10.1039/c5dt01218j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C38 H46 Gd2 N8 O14'
_chemical_formula_weight         1153.33
_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           SHELXL-97
_audit_update_record
;
2014-12-17 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3327(2)
_cell_length_b                   14.0747(3)
_cell_length_c                   12.6772(2)
_cell_measurement_reflns_used    30960
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.87
_cell_measurement_theta_min      6.99
_cell_volume                     2199.97(7)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37020
_diffrn_reflns_theta_full        64.96
_diffrn_reflns_theta_max         64.96
_diffrn_reflns_theta_min         6.99
_exptl_absorpt_coefficient_mu    19.917
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0404P)²+4.4714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3444
_reflns_number_total             3711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01218j2.cif
_cod_data_source_block           pena47
_cod_depositor_comments
'Adding full bibliography for 7035003--7035004.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7035003
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
Gd1 Gd 0.918703(19) 0.110592(17) 0.029085(16) 0.01620(11) Uani 1 1 d .
N1 N 0.8902(3) 0.1282(3) -0.1691(3) 0.0206(8) Uani 1 1 d .
O1 O 1.0620(2) 0.0509(2) -0.0705(2) 0.0187(6) Uani 1 1 d .
O2 O 0.7463(2) 0.0744(3) -0.0093(2) 0.0271(7) Uani 1 1 d .
C1 C 1.0788(4) 0.0892(3) -0.1656(3) 0.0181(9) Uani 1 1 d .
C2 C 1.1813(4) 0.0887(4) -0.2107(4) 0.0270(11) Uani 1 1 d .
C3 C 1.1962(5) 0.1264(4) -0.3099(4) 0.0314(12) Uani 1 1 d .
C4 C 1.1105(5) 0.1657(4) -0.3663(4) 0.0331(12) Uani 1 1 d .
C5 C 1.0081(4) 0.1677(4) -0.3236(4) 0.0288(11) Uani 1 1 d .
C6 C 0.9907(4) 0.1286(3) -0.2225(3) 0.0207(10) Uani 1 1 d .
C7 C 0.8004(4) 0.1366(3) -0.2211(4) 0.0230(10) Uani 1 1 d .
C8 C 0.6936(4) 0.1353(3) -0.1785(4) 0.0240(10) Uani 1 1 d .
C9 C 0.6063(4) 0.1609(4) -0.2470(4) 0.0327(12) Uani 1 1 d .
C10 C 0.5014(4) 0.1610(4) -0.2148(5) 0.0396(13) Uani 1 1 d .
C11 C 0.4795(5) 0.1352(5) -0.1106(5) 0.0400(13) Uani 1 1 d .
C12 C 0.5610(5) 0.1079(4) -0.0436(4) 0.0315(12) Uani 1 1 d .
C13 C 0.6709(4) 0.1058(3) -0.0739(4) 0.0231(10) Uani 1 1 d .
N2 N 0.9413(4) 0.3156(3) 0.0001(3) 0.0282(9) Uani 1 1 d .
O3 O 1.0218(3) 0.2591(2) 0.0012(3) 0.0322(8) Uani 1 1 d .
O4 O 0.8489(3) 0.2771(2) 0.0096(3) 0.0321(8) Uani 1 1 d .
O5 O 0.9516(4) 0.4006(3) -0.0097(4) 0.0502(12) Uani 1 1 d .
O6 O 1.0677(3) 0.1061(2) 0.1580(3) 0.0295(8) Uani 1 1 d .
N3 N 1.2348(4) 0.1046(3) 0.2333(4) 0.0315(10) Uani 1 1 d .
C14 C 1.1677(5) 0.1079(3) 0.1501(4) 0.0292(12) Uani 1 1 d .
C15 C 1.3522(5) 0.1069(4) 0.2222(6) 0.0485(17) Uani 1 1 d .
H15A H 1.3819 0.1628 0.2586 0.073 Uiso 1 1 calc R
H15B H 1.3697 0.1099 0.1472 0.073 Uiso 1 1 calc R
H15C H 1.3841 0.0493 0.2534 0.073 Uiso 1 1 calc R
C16 C 1.1915(6) 0.0975(4) 0.3393(4) 0.0453(16) Uani 1 1 d .
H16A H 1.2497 0.0793 0.3892 0.068 Uiso 1 1 calc R
H16B H 1.1340 0.0494 0.3399 0.068 Uiso 1 1 calc R
H16C H 1.1616 0.1591 0.3600 0.068 Uiso 1 1 calc R
N4 N 0.7554(4) 0.1197(3) 0.3443(3) 0.0325(11) Uani 1 1 d .
O7 O 0.8436(3) 0.1434(3) 0.1935(2) 0.0328(8) Uani 1 1 d .
C17 C 0.8423(5) 0.1306(4) 0.2891(4) 0.0372(13) Uani 1 1 d .
C18 C 0.7597(7) 0.1029(6) 0.4577(5) 0.072(3) Uani 1 1 d .
H18A H 0.7181 0.1522 0.4934 0.108 Uiso 1 1 calc R
H18B H 0.8353 0.1047 0.4831 0.108 Uiso 1 1 calc R
H18C H 0.7285 0.0404 0.4729 0.108 Uiso 1 1 calc R
C19 C 0.6477(5) 0.1207(5) 0.2938(6) 0.0517(18) Uani 1 1 d .
H19A H 0.6066 0.0651 0.3167 0.078 Uiso 1 1 calc R
H19B H 0.6549 0.1190 0.2170 0.078 Uiso 1 1 calc R
H19C H 0.6094 0.1787 0.3139 0.078 Uiso 1 1 calc R
H2 H 1.233(5) 0.066(4) -0.170(5) 0.042(17) Uiso 1 1 d .
H3 H 1.255(5) 0.128(4) -0.334(5) 0.033(16) Uiso 1 1 d .
H4 H 1.118(4) 0.195(4) -0.428(4) 0.026(13) Uiso 1 1 d .
H5 H 0.942(4) 0.198(4) -0.357(4) 0.033(14) Uiso 1 1 d .
H7 H 0.799(4) 0.145(4) -0.289(4) 0.021(13) Uiso 1 1 d .
H9 H 0.623(5) 0.184(4) -0.316(5) 0.045(17) Uiso 1 1 d .
H10 H 0.434(5) 0.174(4) -0.259(4) 0.042(16) Uiso 1 1 d .
H11 H 0.401(5) 0.133(4) -0.085(4) 0.027(14) Uiso 1 1 d .
H13 H 0.549(6) 0.089(4) 0.023(6) 0.052(19) Uiso 1 1 d .
H14 H 1.199(4) 0.119(3) 0.071(4) 0.020(13) Uiso 1 1 d .
H17 H 0.919(5) 0.128(4) 0.341(4) 0.032(15) Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 '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 Gd1 O1 85.35(12) . 3_755
O2 Gd1 O7 81.10(12) . .
O1 Gd1 O7 91.85(11) 3_755 .
O2 Gd1 O1 121.74(11) . .
O1 Gd1 O1 72.52(11) 3_755 .
O7 Gd1 O1 149.81(12) . .
O2 Gd1 O6 147.45(12) . .
O1 Gd1 O6 75.68(11) 3_755 .
O7 Gd1 O6 73.47(13) . .
O1 Gd1 O6 77.62(11) . .
O2 Gd1 O3 130.68(12) . .
O1 Gd1 O3 143.21(11) 3_755 .
O7 Gd1 O3 100.06(12) . .
O1 Gd1 O3 80.24(11) . .
O6 Gd1 O3 74.67(11) . .
O2 Gd1 O4 82.44(12) . .
O1 Gd1 O4 164.08(10) 3_755 .
O7 Gd1 O4 76.22(12) . .
O1 Gd1 O4 122.82(10) . .
O6 Gd1 O4 110.07(11) . .
O3 Gd1 O4 51.16(11) . .
O2 Gd1 N1 72.31(12) . .
O1 Gd1 N1 109.09(11) 3_755 .
O7 Gd1 N1 144.15(13) . .
O1 Gd1 N1 65.99(11) . .
O6 Gd1 N1 138.83(12) . .
O3 Gd1 N1 80.61(12) . .
O4 Gd1 N1 76.81(11) . .
O2 Gd1 N2 106.94(12) . .
O1 Gd1 N2 167.43(11) 3_755 .
O7 Gd1 N2 87.58(12) . .
O1 Gd1 N2 102.15(11) . .
O6 Gd1 N2 92.16(11) . .
O3 Gd1 N2 25.56(11) . .
O4 Gd1 N2 25.61(11) . .
N1 Gd1 N2 77.94(11) . .
O2 Gd1 Gd1 106.04(9) . 3_755
O1 Gd1 Gd1 36.30(7) 3_755 3_755
O7 Gd1 Gd1 123.82(9) . 3_755
O1 Gd1 Gd1 36.21(7) . 3_755
O6 Gd1 Gd1 73.36(8) . 3_755
O3 Gd1 Gd1 113.01(8) . 3_755
O4 Gd1 Gd1 158.76(7) . 3_755
N1 Gd1 Gd1 87.14(9) . 3_755
N2 Gd1 Gd1 137.33(8) . 3_755
C7 N1 C6 120.3(4) . .
C7 N1 Gd1 128.1(3) . .
C6 N1 Gd1 111.5(3) . .
C1 O1 Gd1 125.0(3) . 3_755
C1 O1 Gd1 118.2(3) . .
Gd1 O1 Gd1 107.48(11) 3_755 .
C13 O2 Gd1 136.4(3) . .
O1 C1 C2 121.6(4) . .
O1 C1 C6 119.1(4) . .
C2 C1 C6 119.2(4) . .
C3 C2 C1 120.6(5) . .
C3 C2 H2 125(4) . .
C1 C2 H2 115(4) . .
C4 C3 C2 120.8(5) . .
C4 C3 H3 119(4) . .
C2 C3 H3 120(4) . .
C3 C4 C5 120.0(5) . .
C3 C4 H4 123(3) . .
C5 C4 H4 117(3) . .
C4 C5 C6 120.3(5) . .
C4 C5 H5 125(3) . .
C6 C5 H5 114(3) . .
C1 C6 C5 119.1(4) . .
C1 C6 N1 115.2(4) . .
C5 C6 N1 125.7(4) . .
N1 C7 C8 126.5(4) . .
N1 C7 H7 121(3) . .
C8 C7 H7 112(3) . .
C9 C8 C13 119.0(5) . .
C9 C8 C7 117.2(4) . .
C13 C8 C7 123.8(4) . .
C10 C9 C8 122.0(5) . .
C10 C9 H9 120(4) . .
C8 C9 H9 118(4) . .
C9 C10 C11 119.1(5) . .
C9 C10 H10 127(3) . .
C11 C10 H10 114(3) . .
C12 C11 C10 120.5(5) . .
C12 C11 H11 119(3) . .
C10 C11 H11 121(3) . .
C11 C12 C13 122.4(5) . .
C11 C12 H13 123(4) . .
C13 C12 H13 115(4) . .
O2 C13 C12 120.7(5) . .
O2 C13 C8 122.1(4) . .
C12 C13 C8 117.1(5) . .
O5 N2 O4 121.9(4) . .
O5 N2 O3 122.4(5) . .
O4 N2 O3 115.7(4) . .
O5 N2 Gd1 178.6(4) . .
O4 N2 Gd1 58.6(2) . .
O3 N2 Gd1 57.1(2) . .
N2 O3 Gd1 97.3(3) . .
N2 O4 Gd1 95.8(3) . .
C14 O6 Gd1 133.1(3) . .
C14 N3 C15 121.8(5) . .
C14 N3 C16 119.9(5) . .
C15 N3 C16 118.3(5) . .
O6 C14 N3 122.6(5) . .
O6 C14 H14 117(3) . .
N3 C14 H14 120(3) . .
N3 C15 H15A 109.5 . .
N3 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N3 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N3 C16 H16A 109.5 . .
N3 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N3 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C17 N4 C18 122.6(6) . .
C17 N4 C19 120.9(5) . .
C18 N4 C19 116.5(5) . .
C17 O7 Gd1 149.7(4) . .
O7 C17 N4 125.4(6) . .
O7 C17 H17 123(3) . .
N4 C17 H17 112(3) . .
N4 C18 H18A 109.5 . .
N4 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N4 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N4 C19 H19A 109.5 . .
N4 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
N4 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O2 2.229(3) .
Gd1 O1 2.344(3) 3_755
Gd1 O7 2.346(3) .
Gd1 O1 2.349(3) .
Gd1 O6 2.434(3) .
Gd1 O3 2.476(3) .
Gd1 O4 2.507(3) .
Gd1 N1 2.541(4) .
Gd1 N2 2.923(4) .
Gd1 Gd1 3.7843(5) 3_755
N1 C7 1.282(6) .
N1 C6 1.425(6) .
O1 C1 1.341(5) .
O1 Gd1 2.344(3) 3_755
O2 C13 1.303(6) .
C1 C2 1.399(6) .
C1 C6 1.406(7) .
C2 C3 1.381(7) .
C2 H2 0.87(6) .
C3 C4 1.378(8) .
C3 H3 0.80(6) .
C4 C5 1.385(7) .
C4 H4 0.88(5) .
C5 C6 1.415(6) .
C5 H5 1.00(5) .
C7 C8 1.435(7) .
C7 H7 0.86(5) .
C8 C9 1.415(7) .
C8 C13 1.423(7) .
C9 C10 1.365(8) .
C9 H9 0.96(6) .
C10 C11 1.402(8) .
C10 H10 1.01(6) .
C11 C12 1.358(8) .
C11 H11 1.03(5) .
C12 C13 1.418(7) .
C12 H13 0.90(7) .
N2 O5 1.210(5) .
N2 O4 1.270(5) .
N2 O3 1.271(5) .
O6 C14 1.239(7) .
N3 C14 1.327(7) .
N3 C15 1.458(8) .
N3 C16 1.461(7) .
C14 H14 1.09(5) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
N4 C17 1.302(7) .
N4 C18 1.456(7) .
N4 C19 1.462(8) .
O7 C17 1.225(6) .
C17 H17 1.14(6) .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
