#------------------------------------------------------------------------------
#$Date: 2017-11-02 06:09:32 +0200 (Thu, 02 Nov 2017) $
#$Revision: 202512 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/46/7044618.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_7044618
loop_
_publ_author_name
'Machata, Marek'
'Herchel, Radovan'
'Nemec, Ivan'
'Travnicek, Zdenek'
_publ_section_title
;
 Crystal structures and magnetic properties of two series of phenoxo-O
 bridged dinuclear Ln2 (Ln = Gd, Tb, Dy) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03441E
_journal_year                    2017
_chemical_formula_sum            'C64 H58 Gd2 N4 O12'
_chemical_formula_weight         1389.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2606(13)
_cell_length_b                   15.9046(15)
_cell_length_c                   15.5822(17)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3352
_cell_measurement_theta_min      2.4750
_cell_volume                     2770.5(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40304
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.417
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    2.443
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       prism
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0116P)²+7.0925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             5677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03441e2.cif
_cod_data_source_block           Gd_DMF
_cod_database_code               7044618
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Gd1 Gd 0.52127(2) 0.38808(2) 0.54311(2) 0.01571(6) Uani 1 1 d . .
O1 O 0.6269(2) 0.51118(16) 0.51427(16) 0.0168(6) Uani 1 1 d . .
O2 O 0.5448(2) 0.24826(17) 0.5552(2) 0.0295(7) Uani 1 1 d . .
O3 O 0.6610(2) 0.67351(17) 0.54167(18) 0.0252(7) Uani 1 1 d . .
O4 O 0.6098(2) 0.43686(17) 0.67658(17) 0.0209(6) Uani 1 1 d . .
O5 O 0.3805(2) 0.37873(18) 0.64203(16) 0.0216(6) Uani 1 1 d . .
O6 O 0.5556(3) 0.36553(18) 0.39362(18) 0.0293(7) Uani 1 1 d . .
N1 N 0.7378(3) 0.3431(2) 0.5425(2) 0.0185(7) Uani 1 1 d . .
N2 N 0.6783(4) 0.3268(2) 0.2959(2) 0.0350(9) Uani 1 1 d . .
C1 C 0.7371(3) 0.5356(2) 0.5446(2) 0.0187(9) Uani 1 1 d . .
C2 C 0.7603(3) 0.6219(3) 0.5586(2) 0.0210(9) Uani 1 1 d . .
C3 C 0.8725(4) 0.6531(3) 0.5865(3) 0.0299(10) Uani 1 1 d . .
H3 H 0.8842 0.7119 0.5945 0.036 Uiso 1 1 calc R U
C4 C 0.9682(4) 0.5982(3) 0.6028(3) 0.0354(11) Uani 1 1 d . .
H4 H 1.0460 0.6190 0.6217 0.043 Uiso 1 1 calc R U
C5 C 0.9493(4) 0.5138(3) 0.5913(3) 0.0309(10) Uani 1 1 d . .
H5 H 1.0153 0.4765 0.6025 0.037 Uiso 1 1 calc R U
C6 C 0.8354(3) 0.4804(3) 0.5634(3) 0.0219(9) Uani 1 1 d . .
C7 C 0.8316(3) 0.3889(3) 0.5549(2) 0.0228(8) Uani 1 1 d . .
H7 H 0.9064 0.3606 0.5589 0.027 Uiso 1 1 calc R U
C8 C 0.7485(4) 0.2545(3) 0.5291(3) 0.0216(9) Uani 1 1 d . .
C9 C 0.8502(4) 0.2138(3) 0.5081(3) 0.0279(10) Uani 1 1 d . .
H9 H 0.9214 0.2449 0.5043 0.033 Uiso 1 1 calc R U
C10 C 0.8483(4) 0.1282(3) 0.4925(3) 0.0327(11) Uani 1 1 d . .
H10 H 0.9189 0.1003 0.4801 0.039 Uiso 1 1 calc R U
C11 C 0.7439(4) 0.0832(3) 0.4951(3) 0.0301(11) Uani 1 1 d . .
H11 H 0.7425 0.0247 0.4827 0.036 Uiso 1 1 calc R U
C12 C 0.6413(4) 0.1225(3) 0.5154(3) 0.0279(10) Uani 1 1 d . .
H12 H 0.5701 0.0907 0.5168 0.034 Uiso 1 1 calc R U
C13 C 0.6412(4) 0.2091(2) 0.5340(3) 0.0226(9) Uani 1 1 d . .
C14 C 0.6597(5) 0.7471(3) 0.5956(3) 0.0426(13) Uani 1 1 d . .
H14A H 0.7213 0.7867 0.5815 0.064 Uiso 1 1 calc R U
H14B H 0.6759 0.7307 0.6565 0.064 Uiso 1 1 calc R U
H14C H 0.5810 0.7741 0.5854 0.064 Uiso 1 1 calc R U
C15 C 0.3682(3) 0.4100(2) 0.7154(3) 0.0181(9) Uani 1 1 d . .
C16 C 0.2486(3) 0.3951(2) 0.7471(2) 0.0179(8) Uani 1 1 d . .
C17 C 0.1698(4) 0.3399(3) 0.7016(3) 0.0264(10) Uani 1 1 d . .
H17 H 0.1911 0.3143 0.6505 0.032 Uiso 1 1 calc R U
C18 C 0.0599(4) 0.3211(3) 0.7292(3) 0.0313(10) Uani 1 1 d . .
H18 H 0.0076 0.2819 0.6979 0.038 Uiso 1 1 calc R U
C19 C 0.0268(4) 0.3596(3) 0.8024(3) 0.0289(10) Uani 1 1 d . .
H19 H -0.0486 0.3476 0.8212 0.035 Uiso 1 1 calc R U
C20 C 0.1039(4) 0.4155(3) 0.8475(3) 0.0300(10) Uani 1 1 d . .
H20 H 0.0811 0.4424 0.8974 0.036 Uiso 1 1 calc R U
C21 C 0.2142(4) 0.4330(3) 0.8212(3) 0.0267(10) Uani 1 1 d . .
H21 H 0.2670 0.4710 0.8536 0.032 Uiso 1 1 calc R U
C22 C 0.4561(3) 0.4576(2) 0.7644(3) 0.0203(9) Uani 1 1 d . .
H22 H 0.4372 0.4816 0.8169 0.024 Uiso 1 1 calc R U
C23 C 0.5707(3) 0.4718(2) 0.7405(2) 0.0174(8) Uani 1 1 d . .
C24 C 0.6555(4) 0.5296(2) 0.7931(3) 0.0193(9) Uani 1 1 d . .
C25 C 0.6156(4) 0.5941(3) 0.8422(3) 0.0292(10) Uani 1 1 d . .
H25 H 0.5322 0.6015 0.8438 0.035 Uiso 1 1 calc R U
C26 C 0.6962(4) 0.6481(3) 0.8892(3) 0.0354(11) Uani 1 1 d . .
H26 H 0.6679 0.6925 0.9221 0.042 Uiso 1 1 calc R U
C27 C 0.8183(4) 0.6366(3) 0.8876(3) 0.0326(11) Uani 1 1 d . .
H27 H 0.8738 0.6719 0.9212 0.039 Uiso 1 1 calc R U
C28 C 0.8591(4) 0.5735(3) 0.8371(3) 0.0278(10) Uani 1 1 d . .
H28 H 0.9425 0.5665 0.8350 0.033 Uiso 1 1 calc R U
C29 C 0.7784(4) 0.5209(3) 0.7900(3) 0.0224(9) Uani 1 1 d . .
H29 H 0.8068 0.4782 0.7550 0.027 Uiso 1 1 calc R U
C30 C 0.6403(4) 0.3789(3) 0.3543(3) 0.0265(9) Uani 1 1 d . .
H30 H 0.6828 0.4300 0.3659 0.032 Uiso 1 1 calc R U
C31 C 0.6196(5) 0.2469(3) 0.2776(3) 0.0525(16) Uani 1 1 d . .
H31A H 0.5645 0.2514 0.2241 0.079 Uiso 1 1 calc R U
H31B H 0.5748 0.2316 0.3254 0.079 Uiso 1 1 calc R U
H31C H 0.6797 0.2037 0.2707 0.079 Uiso 1 1 calc R U
C32 C 0.7744(5) 0.3507(4) 0.2463(3) 0.0448(13) Uani 1 1 d . .
H32A H 0.7432 0.3551 0.1850 0.067 Uiso 1 1 calc R U
H32B H 0.8376 0.3080 0.2536 0.067 Uiso 1 1 calc R U
H32C H 0.8073 0.4051 0.2668 0.067 Uiso 1 1 calc R U
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'
Gd Gd -0.1653 3.9035 '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'
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 O4 102.80(10) . .
O2 Gd1 O5 87.95(10) . .
O4 Gd1 O5 71.61(9) . .
O2 Gd1 O1 141.28(9) . .
O4 Gd1 O1 73.89(9) . .
O5 Gd1 O1 124.98(9) . .
O2 Gd1 O1 139.50(9) . 3_666
O4 Gd1 O1 108.25(9) . 3_666
O5 Gd1 O1 78.07(9) . 3_666
O1 Gd1 O1 73.72(10) . 3_666
O2 Gd1 O6 84.47(11) . .
O4 Gd1 O6 143.51(10) . .
O5 Gd1 O6 144.86(9) . .
O1 Gd1 O6 78.37(9) . .
O1 Gd1 O6 85.71(9) 3_666 .
O2 Gd1 O3 74.79(10) . 3_666
O4 Gd1 O3 146.88(9) . 3_666
O5 Gd1 O3 75.28(9) . 3_666
O1 Gd1 O3 128.58(9) . 3_666
O1 Gd1 O3 64.95(9) 3_666 3_666
O6 Gd1 O3 69.61(10) . 3_666
O2 Gd1 N1 67.55(10) . .
O4 Gd1 N1 77.84(10) . .
O5 Gd1 N1 135.16(9) . .
O1 Gd1 N1 74.18(10) . .
O1 Gd1 N1 143.92(9) 3_666 .
O6 Gd1 N1 72.07(10) . .
O3 Gd1 N1 127.88(10) 3_666 .
O2 Gd1 Gd1 164.28(8) . 3_666
O4 Gd1 Gd1 91.48(7) . 3_666
O5 Gd1 Gd1 102.97(7) . 3_666
O1 Gd1 Gd1 37.26(6) . 3_666
O1 Gd1 Gd1 36.46(6) 3_666 3_666
O6 Gd1 Gd1 80.10(7) . 3_666
O3 Gd1 Gd1 96.84(7) 3_666 3_666
N1 Gd1 Gd1 109.94(7) . 3_666
C1 O1 Gd1 130.0(2) . .
C1 O1 Gd1 120.9(2) . 3_666
Gd1 O1 Gd1 106.28(10) . 3_666
C13 O2 Gd1 122.4(2) . .
C2 O3 C14 115.7(3) . .
C2 O3 Gd1 117.4(2) . 3_666
C14 O3 Gd1 124.0(3) . 3_666
C23 O4 Gd1 134.3(2) . .
C15 O5 Gd1 136.3(2) . .
C30 O6 Gd1 133.0(3) . .
C7 N1 C8 120.0(3) . .
C7 N1 Gd1 127.9(3) . .
C8 N1 Gd1 112.0(2) . .
C30 N2 C31 120.2(4) . .
C30 N2 C32 121.2(4) . .
C31 N2 C32 118.5(4) . .
O1 C1 C2 119.1(3) . .
O1 C1 C6 124.4(4) . .
C2 C1 C6 116.5(4) . .
C3 C2 O3 122.3(4) . .
C3 C2 C1 123.1(4) . .
O3 C2 C1 114.6(3) . .
C2 C3 C4 119.6(4) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
C5 C4 C3 119.3(4) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C4 C5 C6 122.1(4) . .
C4 C5 H5 118.9 . .
C6 C5 H5 118.9 . .
C5 C6 C1 119.4(4) . .
C5 C6 C7 114.8(4) . .
C1 C6 C7 125.8(4) . .
N1 C7 C6 126.5(4) . .
N1 C7 H7 116.7 . .
C6 C7 H7 116.7 . .
C9 C8 C13 120.5(4) . .
C9 C8 N1 125.5(4) . .
C13 C8 N1 114.0(3) . .
C10 C9 C8 120.4(4) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C11 C10 C9 120.0(4) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.7(4) . .
C10 C11 H11 119.7 . .
C12 C11 H11 119.7 . .
C11 C12 C13 120.7(4) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
O2 C13 C12 122.1(4) . .
O2 C13 C8 120.2(4) . .
C12 C13 C8 117.8(4) . .
O3 C14 H14A 109.5 . .
O3 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
O3 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O5 C15 C22 123.8(4) . .
O5 C15 C16 115.6(3) . .
C22 C15 C16 120.5(4) . .
C17 C16 C21 118.2(4) . .
C17 C16 C15 118.4(4) . .
C21 C16 C15 123.4(4) . .
C16 C17 C18 121.2(4) . .
C16 C17 H17 119.4 . .
C18 C17 H17 119.4 . .
C19 C18 C17 119.8(4) . .
C19 C18 H18 120.1 . .
C17 C18 H18 120.1 . .
C20 C19 C18 119.4(4) . .
C20 C19 H19 120.3 . .
C18 C19 H19 120.3 . .
C19 C20 C21 120.8(4) . .
C19 C20 H20 119.6 . .
C21 C20 H20 119.6 . .
C20 C21 C16 120.5(4) . .
C20 C21 H21 119.8 . .
C16 C21 H21 119.8 . .
C15 C22 C23 123.8(4) . .
C15 C22 H22 118.1 . .
C23 C22 H22 118.1 . .
O4 C23 C22 123.8(4) . .
O4 C23 C24 116.2(3) . .
C22 C23 C24 120.0(3) . .
C25 C24 C29 118.7(4) . .
C25 C24 C23 121.9(4) . .
C29 C24 C23 119.3(4) . .
C24 C25 C26 120.9(4) . .
C24 C25 H25 119.6 . .
C26 C25 H25 119.6 . .
C27 C26 C25 119.5(4) . .
C27 C26 H26 120.2 . .
C25 C26 H26 120.2 . .
C28 C27 C26 120.1(4) . .
C28 C27 H27 120.0 . .
C26 C27 H27 120.0 . .
C29 C28 C27 119.9(4) . .
C29 C28 H28 120.1 . .
C27 C28 H28 120.1 . .
C28 C29 C24 120.9(4) . .
C28 C29 H29 119.5 . .
C24 C29 H29 119.5 . .
O6 C30 N2 124.7(4) . .
O6 C30 H30 117.6 . .
N2 C30 H30 117.6 . .
N2 C31 H31A 109.5 . .
N2 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
N2 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N2 C32 H32A 109.5 . .
N2 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
N2 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 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 2.245(3) .
Gd1 O4 2.329(3) .
Gd1 O5 2.345(3) .
Gd1 O1 2.362(3) .
Gd1 O1 2.406(3) 3_666
Gd1 O6 2.433(3) .
Gd1 O3 2.503(3) 3_666
Gd1 N1 2.542(3) .
Gd1 Gd1 3.8151(5) 3_666
O1 C1 1.331(5) .
O1 Gd1 2.406(3) 3_666
O2 C13 1.327(5) .
O3 C2 1.386(5) .
O3 C14 1.442(5) .
O3 Gd1 2.503(3) 3_666
O4 C23 1.265(5) .
O5 C15 1.270(5) .
O6 C30 1.212(5) .
N1 C7 1.279(5) .
N1 C8 1.432(5) .
N2 C30 1.339(5) .
N2 C31 1.444(6) .
N2 C32 1.455(6) .
C1 C2 1.410(6) .
C1 C6 1.416(6) .
C2 C3 1.379(5) .
C3 C4 1.387(6) .
C3 H3 0.9500 .
C4 C5 1.368(6) .
C4 H4 0.9500 .
C5 C6 1.408(5) .
C5 H5 0.9500 .
C6 C7 1.461(6) .
C7 H7 0.9500 .
C8 C9 1.389(6) .
C8 C13 1.418(6) .
C9 C10 1.383(6) .
C9 H9 0.9500 .
C10 C11 1.381(6) .
C10 H10 0.9500 .
C11 C12 1.384(6) .
C11 H11 0.9500 .
C12 C13 1.408(6) .
C12 H12 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C22 1.398(5) .
C15 C16 1.507(5) .
C16 C17 1.383(6) .
C16 C21 1.397(5) .
C17 C18 1.391(6) .
C17 H17 0.9500 .
C18 C19 1.385(6) .
C18 H18 0.9500 .
C19 C20 1.376(6) .
C19 H19 0.9500 .
C20 C21 1.382(6) .
C20 H20 0.9500 .
C21 H21 0.9500 .
C22 C23 1.404(5) .
C22 H22 0.9500 .
C23 C24 1.496(5) .
C24 C25 1.386(6) .
C24 C29 1.398(6) .
C25 C26 1.392(6) .
C25 H25 0.9500 .
C26 C27 1.391(6) .
C26 H26 0.9500 .
C27 C28 1.387(6) .
C27 H27 0.9500 .
C28 C29 1.380(6) .
C28 H28 0.9500 .
C29 H29 0.9500 .
C30 H30 0.9500 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
