#------------------------------------------------------------------------------
#$Date: 2020-11-06 13:18:30 +0100 (vie 06 de nov de 2020) $
#$Revision: 258852 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/54/7705457.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_7705457
loop_
_publ_author_name
'Shen, Fu-Xing'
'Pramanik, Kuheli'
'Brandão, Paula'
'Zhang, Yi-Quan'
'Jana, Narayan Ch'
'Wang, Xin-Yi'
'Panja, Anangamohan'
_publ_section_title
;
 Macrocycle supported dimetallic lanthanide complexes with slow magnetic
 relaxation in Dy₂ analogues.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14169
_journal_page_last               14179
_journal_paper_doi               10.1039/d0dt02778b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C42 H52 Cl2 Gd2 N4 O10'
_chemical_formula_weight         1158.27
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-15 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.119(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2419(6)
_cell_length_b                   15.4182(8)
_cell_length_c                   12.3911(6)
_cell_measurement_reflns_used    424
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.98
_cell_volume                     2257.8(2)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Mercury (Macrae et al 2008)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37933
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.145
_diffrn_reflns_theta_min         2.155
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.089
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.642
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0221P)²+3.0470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4019
_reflns_number_total             4989
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02778b2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 7705453--7705458.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7705457
_shelx_shelxl_version_number     2018/3
_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   0.790
_shelx_estimated_absorpt_t_max   0.941
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.51530(2) 0.38802(2) 0.57902(2) 0.03335(6) Uani 1 1 d . . . . .
Cl1 Cl 0.43134(9) 0.29721(7) -0.03420(7) 0.0474(2) Uani 1 1 d . . . . .
O1 O 0.4932(2) 0.45666(15) 0.40745(18) 0.0356(5) Uani 1 1 d . . . . .
O2 O 0.4820(2) 0.25929(16) 0.6680(2) 0.0418(6) Uani 1 1 d . . . . .
O3 O 0.5686(2) 0.27224(18) 0.4832(2) 0.0442(6) Uani 1 1 d . . . . .
O4 O 0.6168(2) 0.40857(17) 0.7657(2) 0.0418(6) Uani 1 1 d . . . . .
O5 O 0.7066(2) 0.40847(19) 0.5818(2) 0.0475(7) Uani 1 1 d . . . . .
N1 N 0.3261(2) 0.3373(2) 0.4392(2) 0.0352(6) Uani 1 1 d . . . . .
N2 N 0.6319(3) 0.5787(2) 0.3074(3) 0.0400(7) Uani 1 1 d . . . . .
C1 C 0.4802(3) 0.4156(2) 0.3108(3) 0.0353(8) Uani 1 1 d . . . . .
C2 C 0.3901(3) 0.3577(2) 0.2689(3) 0.0338(8) Uani 1 1 d . . . . .
C3 C 0.3749(3) 0.3215(2) 0.1623(3) 0.0350(8) Uani 1 1 d . . . . .
H3 H 0.312791 0.283902 0.132711 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4505(3) 0.3408(2) 0.1004(3) 0.0368(8) Uani 1 1 d . . . . .
C5 C 0.5423(3) 0.3940(2) 0.1421(3) 0.0425(9) Uani 1 1 d . . . . .
H5 H 0.594699 0.404922 0.099106 0.051 Uiso 1 1 calc R U . . .
C6 C 0.5583(3) 0.4319(2) 0.2473(3) 0.0382(8) Uani 1 1 d . . . . .
C7 C 0.3115(3) 0.3309(2) 0.3334(3) 0.0373(8) Uani 1 1 d . . . . .
H7 H 0.242128 0.305986 0.292304 0.045 Uiso 1 1 calc R U . . .
C8 C 0.2354(3) 0.2990(3) 0.4821(3) 0.0398(8) Uani 1 1 d . . . . .
H8A H 0.263962 0.245252 0.523577 0.048 Uiso 1 1 calc R U . . .
H8B H 0.171311 0.283015 0.418156 0.048 Uiso 1 1 calc R U . . .
C9 C 0.6606(3) 0.4866(3) 0.2978(3) 0.0460(9) Uani 1 1 d . . . . .
H9A H 0.698385 0.463956 0.373008 0.055 Uiso 1 1 calc R U . . .
H9B H 0.714674 0.481997 0.250988 0.055 Uiso 1 1 calc R U . . .
C10 C 0.7332(3) 0.6344(3) 0.3216(3) 0.0456(10) Uani 1 1 d . . . . .
H10A H 0.708314 0.693700 0.295683 0.055 Uiso 1 1 calc R U . . .
H10B H 0.779543 0.612017 0.273062 0.055 Uiso 1 1 calc R U . . .
C11 C 0.8072(3) 0.6398(3) 0.4410(3) 0.0463(10) Uani 1 1 d . . . . .
H11A H 0.883850 0.658697 0.438744 0.056 Uiso 1 1 calc R U . . .
H11B H 0.814209 0.580913 0.473933 0.056 Uiso 1 1 calc R U . . .
C12 C 0.4898(3) 0.1795(2) 0.6511(3) 0.0379(8) Uani 1 1 d . . . . .
C13 C 0.5307(4) 0.1437(3) 0.5667(3) 0.0495(10) Uani 1 1 d . . . . .
H13 H 0.534155 0.082261 0.562713 0.059 Uiso 1 1 calc R U . . .
C14 C 0.5670(3) 0.1916(3) 0.4875(3) 0.0384(8) Uani 1 1 d . . . . .
C15 C 0.4514(4) 0.1207(3) 0.7321(4) 0.0569(11) Uani 1 1 d . . . . .
H15A H 0.502038 0.127736 0.807160 0.085 Uiso 1 1 calc R U . . .
H15B H 0.453237 0.060231 0.708222 0.085 Uiso 1 1 calc R U . . .
H15C H 0.374043 0.136071 0.733311 0.085 Uiso 1 1 calc R U . . .
C16 C 0.6103(4) 0.1464(3) 0.3982(4) 0.0571(11) Uani 1 1 d . . . . .
H16A H 0.571345 0.169544 0.324601 0.086 Uiso 1 1 calc R U . . .
H16B H 0.595714 0.083951 0.400141 0.086 Uiso 1 1 calc R U . . .
H16C H 0.691884 0.156299 0.412156 0.086 Uiso 1 1 calc R U . . .
C17 C 0.7168(3) 0.4281(3) 0.8162(3) 0.0392(8) Uani 1 1 d . . . . .
C18 C 0.8073(3) 0.4313(3) 0.7679(3) 0.0469(9) Uani 1 1 d . . . . .
H18 H 0.880453 0.442248 0.815612 0.056 Uiso 1 1 calc R U . . .
C19 C 0.7981(3) 0.4195(2) 0.6543(3) 0.0394(8) Uani 1 1 d . . . . .
C20 C 0.7362(4) 0.4490(3) 0.9385(3) 0.0511(10) Uani 1 1 d . . . . .
H20A H 0.696383 0.502682 0.946846 0.077 Uiso 1 1 calc R U . . .
H20B H 0.817441 0.456389 0.972494 0.077 Uiso 1 1 calc R U . . .
H20C H 0.707512 0.401398 0.975875 0.077 Uiso 1 1 calc R U . . .
C21 C 0.9045(3) 0.4180(3) 0.6135(3) 0.0460(9) Uani 1 1 d . . . . .
H21A H 0.891766 0.381976 0.546192 0.069 Uiso 1 1 calc R U . . .
H21B H 0.967029 0.393751 0.671947 0.069 Uiso 1 1 calc R U . . .
H21C H 0.923495 0.477161 0.596042 0.069 Uiso 1 1 calc R U . . .
H2 H 0.590(5) 0.582(4) 0.243(5) 0.086(19) 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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
O1 Gd O3 82.18(9) . . ?
O1 Gd O4 138.20(9) . . ?
O3 Gd O4 117.36(9) . . ?
O1 Gd O5 80.23(9) . . ?
O3 Gd O5 72.56(9) . . ?
O4 Gd O5 72.43(9) . . ?
O1 Gd O2 144.83(8) . . ?
O3 Gd O2 72.46(9) . . ?
O4 Gd O2 76.35(9) . . ?
O5 Gd O2 113.48(10) . . ?
O1 Gd O1 67.29(9) . 3_666 ?
O3 Gd O1 145.26(8) . 3_666 ?
O4 Gd O1 79.52(9) . 3_666 ?
O5 Gd O1 85.81(9) . 3_666 ?
O2 Gd O1 142.19(8) . 3_666 ?
O1 Gd N2 118.11(10) . 3_666 ?
O3 Gd N2 138.60(10) . 3_666 ?
O4 Gd N2 72.80(10) . 3_666 ?
O5 Gd N2 142.15(10) . 3_666 ?
O2 Gd N2 71.69(10) . 3_666 ?
O1 Gd N2 73.60(9) 3_666 3_666 ?
O1 Gd N1 70.13(8) . . ?
O3 Gd N1 75.62(9) . . ?
O4 Gd N1 147.27(8) . . ?
O5 Gd N1 138.86(9) . . ?
O2 Gd N1 80.07(9) . . ?
O1 Gd N1 107.19(9) 3_666 . ?
N2 Gd N1 78.45(10) 3_666 . ?
O1 Gd Gd 34.28(6) . 3_666 ?
O3 Gd Gd 114.92(7) . 3_666 ?
O4 Gd Gd 109.23(6) . 3_666 ?
O5 Gd Gd 81.67(7) . 3_666 ?
O2 Gd Gd 164.83(6) . 3_666 ?
O1 Gd Gd 33.02(5) 3_666 3_666 ?
N2 Gd Gd 96.08(8) 3_666 3_666 ?
N1 Gd Gd 88.84(6) . 3_666 ?
C1 O1 Gd 124.4(2) . . ?
C1 O1 Gd 122.8(2) . 3_666 ?
Gd O1 Gd 112.71(9) . 3_666 ?
C12 O2 Gd 135.9(2) . . ?
C14 O3 Gd 137.2(2) . . ?
C17 O4 Gd 136.1(2) . . ?
C19 O5 Gd 136.8(2) . . ?
C7 N1 C8 114.9(3) . . ?
C7 N1 Gd 124.2(2) . . ?
C8 N1 Gd 120.0(2) . . ?
C9 N2 C10 111.0(3) . . ?
C9 N2 Gd 116.5(2) . 3_666 ?
C10 N2 Gd 119.7(2) . 3_666 ?
C9 N2 H2 95(4) . . ?
C10 N2 H2 111(4) . . ?
Gd N2 H2 100(4) 3_666 . ?
O1 C1 C2 122.2(3) . . ?
O1 C1 C6 118.6(3) . . ?
C2 C1 C6 119.1(3) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C7 117.3(3) . . ?
C1 C2 C7 122.8(3) . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 Cl1 118.5(3) . . ?
C3 C4 Cl1 120.1(3) . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C9 121.5(3) . . ?
C1 C6 C9 118.7(3) . . ?
N1 C7 C2 127.0(3) . . ?
N1 C7 H7 116.5 . . ?
C2 C7 H7 116.5 . . ?
N1 C8 C11 112.9(3) . 3_666 ?
N1 C8 H8A 109.0 . . ?
C11 C8 H8A 109.0 3_666 . ?
N1 C8 H8B 109.0 . . ?
C11 C8 H8B 109.0 3_666 . ?
H8A C8 H8B 107.8 . . ?
N2 C9 C6 112.6(3) . . ?
N2 C9 H9A 109.1 . . ?
C6 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
C6 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 C11 114.5(3) . . ?
N2 C10 H10A 108.6 . . ?
C11 C10 H10A 108.6 . . ?
N2 C10 H10B 108.6 . . ?
C11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C8 115.3(3) . 3_666 ?
C10 C11 H11A 108.5 . . ?
C8 C11 H11A 108.5 3_666 . ?
C10 C11 H11B 108.5 . . ?
C8 C11 H11B 108.5 3_666 . ?
H11A C11 H11B 107.5 . . ?
O2 C12 C13 125.0(4) . . ?
O2 C12 C15 115.2(3) . . ?
C13 C12 C15 119.8(4) . . ?
C12 C13 C14 124.5(4) . . ?
C12 C13 H13 117.8 . . ?
C14 C13 H13 117.8 . . ?
O3 C14 C13 124.9(3) . . ?
O3 C14 C16 114.6(4) . . ?
C13 C14 C16 120.5(4) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 125.2(3) . . ?
O4 C17 C20 115.5(3) . . ?
C18 C17 C20 119.4(4) . . ?
C17 C18 C19 124.4(4) . . ?
C17 C18 H18 117.8 . . ?
C19 C18 H18 117.8 . . ?
O5 C19 C18 124.4(3) . . ?
O5 C19 C21 116.4(3) . . ?
C18 C19 C21 119.2(4) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
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
Gd O1 2.327(2) . ?
Gd O3 2.330(3) . ?
Gd O4 2.345(3) . ?
Gd O5 2.354(3) . ?
Gd O2 2.357(2) . ?
Gd O1 2.405(2) 3_666 ?
Gd N2 2.611(3) 3_666 ?
Gd N1 2.624(3) . ?
Gd Gd 3.9389(4) 3_666 ?
Cl1 C4 1.756(3) . ?
O1 C1 1.327(4) . ?
O2 C12 1.256(4) . ?
O3 C14 1.245(4) . ?
O4 C17 1.257(4) . ?
O5 C19 1.251(5) . ?
N1 C7 1.281(4) . ?
N1 C8 1.473(4) . ?
N2 C9 1.474(5) . ?
N2 C10 1.482(5) . ?
N2 H2 0.83(5) . ?
C1 C2 1.409(5) . ?
C1 C6 1.410(5) . ?
C2 C3 1.401(5) . ?
C2 C7 1.461(5) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(6) . ?
C5 C6 1.395(5) . ?
C5 H5 0.9500 . ?
C6 C9 1.505(5) . ?
C7 H7 0.9500 . ?
C8 C11 1.526(5) 3_666 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.522(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.386(5) . ?
C12 C15 1.515(5) . ?
C13 C14 1.391(6) . ?
C13 H13 0.9500 . ?
C14 C16 1.516(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 . ?
C17 C18 1.391(5) . ?
C17 C20 1.507(5) . ?
C18 C19 1.394(5) . ?
C18 H18 0.9500 . ?
C19 C21 1.516(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
