#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:56 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223713 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/33/7233346.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_7233346
loop_
_publ_author_name
'Kong, Jiao-Jiao'
'Zhang, Jia-Chen'
'Jiang, Yu-Xuan'
'Tao, Jin-Xia'
'Wang, Wen-Yan'
'Huang, Xing-Cai'
_publ_section_title
;
 Two-dimensional heterometallic CuIILnIII (Ln = Tb and Dy) coordination
 polymers bridged by dicyanamides showing slow magnetic relaxation
 behavior
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5145
_journal_paper_doi               10.1039/C9CE00673G
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C27 H24 Cu Gd N11 O4'
_chemical_formula_weight         787.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-20 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.826(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.244(11)
_cell_length_b                   16.166(14)
_cell_length_c                   14.029(12)
_cell_measurement_reflns_used    3552
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.36
_cell_measurement_theta_min      2.28
_cell_volume                     2976(4)
_computing_cell_refinement       'SHELXL-2014/7 (Sheldrick 2014)'
_computing_data_collection       'Bruker Apex D8 QUEST'
_computing_data_reduction        'SHELXL-2014/7 (Sheldrick 2014)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014/7 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Apex D8 QUEST'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37598
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.127
_diffrn_reflns_theta_min         1.932
_exptl_absorpt_coefficient_mu    2.978
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0355P)²+1.3566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5086
_reflns_number_total             7144
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00673g2.cif
_cod_data_source_block           1-CuGd
_cod_depositor_comments
'Adding full bibliography for 7233345--7233347.cif.'
_cod_database_code               7233346
_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.
;
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.574
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.41585(5) 0.07836(4) 0.72186(5) 0.03744(17) Uani 1 1 d . .
Gd1 Gd 0.17842(2) 0.05974(2) 0.79180(2) 0.03451(9) Uani 1 1 d . .
C1 C 0.3946(4) -0.0414(3) 0.8693(4) 0.0362(12) Uani 1 1 d . .
C2 C 0.3318(4) -0.1022(3) 0.9037(4) 0.0426(14) Uani 1 1 d . .
C3 C 0.3734(5) -0.1681(4) 0.9551(4) 0.0515(16) Uani 1 1 d . .
H3 H 0.3314 -0.2092 0.9744 0.062 Uiso 1 1 calc R U
C4 C 0.4784(5) -0.1739(4) 0.9790(5) 0.0590(18) Uani 1 1 d . .
H4 H 0.5064 -0.2176 1.0168 0.071 Uiso 1 1 calc R U
C5 C 0.5405(5) -0.1163(4) 0.9474(4) 0.0534(16) Uani 1 1 d . .
H5 H 0.6108 -0.1213 0.9629 0.064 Uiso 1 1 calc R U
C6 C 0.4992(4) -0.0489(3) 0.8912(4) 0.0430(13) Uani 1 1 d . .
C7 C 0.5696(4) 0.0108(4) 0.8625(4) 0.0462(14) Uani 1 1 d . .
H7 H 0.6369 0.0065 0.8916 0.055 Uiso 1 1 calc R U
C8 C 0.6330(4) 0.1269(4) 0.7904(4) 0.0505(15) Uani 1 1 d . .
H8A H 0.6954 0.1062 0.8268 0.061 Uiso 1 1 calc R U
H8B H 0.6179 0.1797 0.8180 0.061 Uiso 1 1 calc R U
C9 C 0.6513(4) 0.1408(4) 0.6870(4) 0.0444(14) Uani 1 1 d . .
C10 C 0.6696(5) 0.0604(4) 0.6373(5) 0.0661(19) Uani 1 1 d . .
H10A H 0.7257 0.0317 0.6735 0.099 Uiso 1 1 calc R U
H10B H 0.6854 0.0718 0.5738 0.099 Uiso 1 1 calc R U
H10C H 0.6095 0.0267 0.6330 0.099 Uiso 1 1 calc R U
C11 C 0.7450(5) 0.1968(4) 0.6901(5) 0.0657(19) Uani 1 1 d . .
H11A H 0.8023 0.1707 0.7277 0.099 Uiso 1 1 calc R U
H11B H 0.7315 0.2489 0.7188 0.099 Uiso 1 1 calc R U
H11C H 0.7600 0.2058 0.6259 0.099 Uiso 1 1 calc R U
C12 C 0.5632(4) 0.1888(4) 0.6324(5) 0.0536(16) Uani 1 1 d . .
H12A H 0.5566 0.2408 0.6656 0.064 Uiso 1 1 calc R U
H12B H 0.5803 0.2018 0.5690 0.064 Uiso 1 1 calc R U
C13 C 0.4100(4) 0.1550(3) 0.5379(4) 0.0409(13) Uani 1 1 d . .
H13 H 0.4434 0.1775 0.4898 0.049 Uiso 1 1 calc R U
C14 C 0.3043(4) 0.1335(3) 0.5108(4) 0.0358(12) Uani 1 1 d . .
C15 C 0.2613(5) 0.1432(4) 0.4146(4) 0.0488(15) Uani 1 1 d . .
H15 H 0.3031 0.1564 0.3686 0.059 Uiso 1 1 calc R U
C16 C 0.1597(5) 0.1337(4) 0.3873(4) 0.0510(15) Uani 1 1 d . .
H16 H 0.1327 0.1387 0.3227 0.061 Uiso 1 1 calc R U
C17 C 0.0962(5) 0.1166(4) 0.4550(4) 0.0490(15) Uani 1 1 d . .
H17 H 0.0264 0.1113 0.4363 0.059 Uiso 1 1 calc R U
C18 C 0.1358(4) 0.1073(3) 0.5499(4) 0.0386(13) Uani 1 1 d . .
C19 C 0.2406(4) 0.1138(3) 0.5799(4) 0.0344(12) Uani 1 1 d . .
C20 C -0.0295(4) 0.0994(4) 0.6034(5) 0.0524(16) Uani 1 1 d . .
H20A H -0.0481 0.1530 0.5772 0.079 Uiso 1 1 calc R U
H20B H -0.0595 0.0912 0.6612 0.079 Uiso 1 1 calc R U
H20C H -0.0537 0.0575 0.5573 0.079 Uiso 1 1 calc R U
C21 C 0.1641(6) -0.1556(5) 0.8933(8) 0.113(4) Uani 1 1 d . .
H21A H 0.1913 -0.2063 0.8720 0.170 Uiso 1 1 calc R U
H21B H 0.0980 -0.1458 0.8577 0.170 Uiso 1 1 calc R U
H21C H 0.1582 -0.1596 0.9606 0.170 Uiso 1 1 calc R U
C22 C 0.4588(5) -0.1147(4) 0.6621(5) 0.0518(16) Uani 1 1 d . .
C23 C 0.1831(5) -0.1157(4) 0.6381(5) 0.0521(16) Uani 1 1 d . .
C24 C 0.2926(5) 0.2474(4) 0.8796(4) 0.0486(15) Uani 1 1 d . .
C25 C 0.0371(5) 0.2462(4) 0.8099(5) 0.0528(16) Uani 1 1 d . .
C26 C 0.1519(5) 0.0603(5) 1.0428(5) 0.0614(19) Uani 1 1 d . .
C27 C -0.0566(5) -0.0268(5) 0.8403(5) 0.0603(18) Uani 1 1 d . .
O1 O 0.3497(3) 0.0210(2) 0.8194(3) 0.0387(9) Uani 1 1 d . .
O2 O 0.2748(3) 0.1039(2) 0.6730(3) 0.0367(8) Uani 1 1 d . .
O3 O 0.2301(3) -0.0892(2) 0.8780(3) 0.0572(12) Uani 1 1 d . .
O4 O 0.0798(3) 0.0940(2) 0.6249(3) 0.0446(9) Uani 1 1 d . .
N1 N 0.5500(3) 0.0690(3) 0.8015(3) 0.0436(11) Uani 1 1 d . .
N2 N 0.4631(3) 0.1465(3) 0.6207(3) 0.0375(10) Uani 1 1 d . .
N3 N 0.4287(4) -0.0493(3) 0.6449(4) 0.0593(14) Uani 1 1 d . .
N4 N 0.2825(4) 0.1814(3) 0.8561(4) 0.0521(13) Uani 1 1 d . .
N5 N 0.0666(4) 0.1807(4) 0.8018(4) 0.0675(16) Uani 1 1 d . .
N6 N -0.0059(4) 0.3152(3) 0.8217(5) 0.0748(18) Uani 1 1 d . .
N7 N 0.1741(4) 0.0638(4) 0.9676(4) 0.0639(15) Uani 1 1 d . .
N8 N 0.1704(4) -0.0578(3) 0.6794(4) 0.0561(14) Uani 1 1 d . .
N9 N 0.1964(5) -0.1787(3) 0.5817(4) 0.083(2) Uani 1 1 d . .
N10 N 0.0109(4) -0.0034(3) 0.8084(4) 0.0548(14) Uani 1 1 d . .
N11 N -0.1369(5) -0.0597(6) 0.8671(5) 0.121(3) 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'
Cu Cu 0.3201 1.2651 '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
O2 Cu1 O1 81.19(15) . .
O2 Cu1 N2 90.64(17) . .
O1 Cu1 N2 171.09(16) . .
O2 Cu1 N1 164.65(18) . .
O1 Cu1 N1 91.25(18) . .
N2 Cu1 N1 95.8(2) . .
O2 Cu1 N3 98.69(18) . .
O1 Cu1 N3 88.43(18) . .
N2 Cu1 N3 96.4(2) . .
N1 Cu1 N3 94.4(2) . .
O2 Cu1 Gd1 41.05(11) . .
O1 Cu1 Gd1 40.84(10) . .
N2 Cu1 Gd1 130.51(13) . .
N1 Cu1 Gd1 128.39(15) . .
N3 Cu1 Gd1 100.44(14) . .
O1 Gd1 O2 65.71(13) . .
O1 Gd1 N8 81.68(15) . .
O2 Gd1 N8 76.10(16) . .
O1 Gd1 N5 141.24(16) . .
O2 Gd1 N5 100.83(17) . .
N8 Gd1 N5 132.39(18) . .
O1 Gd1 N7 89.76(16) . .
O2 Gd1 N7 142.09(16) . .
N8 Gd1 N7 130.82(19) . .
N5 Gd1 N7 80.0(2) . .
O1 Gd1 N10 137.34(16) . .
O2 Gd1 N10 140.55(15) . .
N8 Gd1 N10 77.41(18) . .
N5 Gd1 N10 76.68(19) . .
N7 Gd1 N10 76.99(18) . .
O1 Gd1 N4 71.06(15) . .
O2 Gd1 N4 71.94(15) . .
N8 Gd1 N4 144.30(18) . .
N5 Gd1 N4 70.20(19) . .
N7 Gd1 N4 72.90(17) . .
N10 Gd1 N4 138.24(17) . .
O1 Gd1 O4 124.62(12) . .
O2 Gd1 O4 63.05(13) . .
N8 Gd1 O4 67.19(16) . .
N5 Gd1 O4 69.41(17) . .
N7 Gd1 O4 145.14(17) . .
N10 Gd1 O4 79.93(15) . .
N4 Gd1 O4 110.15(15) . .
O1 Gd1 O3 60.83(12) . .
O2 Gd1 O3 117.02(13) . .
N8 Gd1 O3 65.84(17) . .
N5 Gd1 O3 141.90(18) . .
N7 Gd1 O3 67.78(17) . .
N10 Gd1 O3 76.69(15) . .
N4 Gd1 O3 116.13(16) . .
O4 Gd1 O3 130.86(13) . .
O1 Gd1 Cu1 33.22(9) . .
O2 Gd1 Cu1 33.02(8) . .
N8 Gd1 Cu1 81.13(13) . .
N5 Gd1 Cu1 121.78(15) . .
N7 Gd1 Cu1 115.39(14) . .
N10 Gd1 Cu1 158.20(13) . .
N4 Gd1 Cu1 63.41(12) . .
O4 Gd1 Cu1 95.27(10) . .
O3 Gd1 Cu1 91.14(9) . .
O1 C1 C6 123.3(5) . .
O1 C1 C2 118.0(5) . .
C6 C1 C2 118.7(5) . .
C3 C2 O3 125.1(5) . .
C3 C2 C1 120.7(6) . .
O3 C2 C1 114.1(5) . .
C2 C3 C4 120.0(6) . .
C5 C4 C3 120.5(6) . .
C4 C5 C6 120.5(6) . .
C1 C6 C5 119.4(5) . .
C1 C6 C7 123.2(5) . .
C5 C6 C7 117.3(5) . .
N1 C7 C6 127.1(5) . .
N1 C8 C9 114.5(5) . .
C10 C9 C12 111.6(5) . .
C10 C9 C8 111.7(5) . .
C12 C9 C8 110.3(5) . .
C10 C9 C11 109.9(5) . .
C12 C9 C11 106.0(5) . .
C8 C9 C11 107.1(5) . .
N2 C12 C9 115.8(5) . .
N2 C13 C14 127.4(5) . .
C15 C14 C19 119.1(5) . .
C15 C14 C13 118.7(5) . .
C19 C14 C13 121.7(5) . .
C16 C15 C14 121.2(6) . .
C15 C16 C17 120.1(6) . .
C18 C17 C16 120.2(6) . .
C17 C18 O4 125.6(5) . .
C17 C18 C19 121.1(5) . .
O4 C18 C19 113.3(5) . .
O2 C19 C18 118.5(5) . .
O2 C19 C14 123.2(5) . .
C18 C19 C14 118.3(5) . .
N3 C22 N6 171.3(7) . 2_546
N8 C23 N9 174.1(7) . .
N4 C24 N9 172.7(7) . 2_556
N5 C25 N6 172.9(8) . .
N7 C26 N11 173.4(7) . 3_557
N10 C27 N11 172.6(8) . .
C1 O1 Cu1 121.4(3) . .
C1 O1 Gd1 130.4(3) . .
Cu1 O1 Gd1 105.95(15) . .
C19 O2 Cu1 123.6(3) . .
C19 O2 Gd1 126.0(3) . .
Cu1 O2 Gd1 105.93(16) . .
C2 O3 C21 116.8(5) . .
C2 O3 Gd1 115.5(3) . .
C21 O3 Gd1 127.6(4) . .
C18 O4 C20 117.2(4) . .
C18 O4 Gd1 117.8(3) . .
C20 O4 Gd1 125.0(3) . .
C7 N1 C8 117.0(5) . .
C7 N1 Cu1 121.5(4) . .
C8 N1 Cu1 121.4(4) . .
C13 N2 C12 115.1(5) . .
C13 N2 Cu1 121.7(4) . .
C12 N2 Cu1 123.1(4) . .
C22 N3 Cu1 139.6(5) . .
C24 N4 Gd1 153.5(5) . .
C25 N5 Gd1 163.4(5) . .
C25 N6 C22 125.1(6) . 2_556
C26 N7 Gd1 165.8(5) . .
C23 N8 Gd1 167.2(5) . .
C24 N9 C23 118.2(6) 2_546 .
C27 N10 Gd1 161.9(5) . .
C27 N11 C26 121.7(6) . 3_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.945(4) .
Cu1 O1 1.955(4) .
Cu1 N2 1.965(5) .
Cu1 N1 1.972(5) .
Cu1 N3 2.345(6) .
Cu1 Gd1 3.432(3) .
Gd1 O1 2.334(4) .
Gd1 O2 2.344(4) .
Gd1 N8 2.461(5) .
Gd1 N5 2.468(6) .
Gd1 N7 2.476(6) .
Gd1 N10 2.481(5) .
Gd1 N4 2.498(5) .
Gd1 O4 2.581(4) .
Gd1 O3 2.739(4) .
C1 O1 1.323(6) .
C1 C6 1.384(8) .
C1 C2 1.414(8) .
C2 C3 1.359(8) .
C2 O3 1.363(7) .
C3 C4 1.389(8) .
C4 C5 1.355(9) .
C5 C6 1.411(8) .
C6 C7 1.437(8) .
C7 N1 1.274(7) .
C8 N1 1.469(7) .
C8 C9 1.519(8) .
C9 C10 1.511(8) .
C9 C12 1.518(8) .
C9 C11 1.532(8) .
C12 N2 1.482(7) .
C13 N2 1.280(7) .
C13 C14 1.441(7) .
C14 C15 1.400(8) .
C14 C19 1.406(7) .
C15 C16 1.357(8) .
C16 C17 1.380(8) .
C17 C18 1.371(8) .
C18 O4 1.384(6) .
C18 C19 1.398(7) .
C19 O2 1.332(6) .
C20 O4 1.441(6) .
C21 O3 1.419(7) .
C22 N3 1.143(8) .
C22 N6 1.299(8) 2_546
C23 N8 1.126(7) .
C23 N9 1.316(8) .
C24 N4 1.119(7) .
C24 N9 1.312(8) 2_556
C25 N5 1.140(7) .
C25 N6 1.273(8) .
C26 N7 1.134(8) .
C26 N11 1.306(9) 3_557
C27 N10 1.119(7) .
C27 N11 1.290(9) .
N6 C22 1.299(8) 2_556
N9 C24 1.312(8) 2_546
N11 C26 1.306(9) 3_557
