#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:18:30 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258852 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/54/7705453.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_7705453
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 Dy2 N4 O10'
_chemical_formula_weight         1168.77
_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                 105.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2038(9)
_cell_length_b                   15.3000(11)
_cell_length_c                   12.3636(10)
_cell_measurement_reflns_used    456
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.90
_cell_volume                     2222.4(3)
_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 0.997
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58354
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.570
_diffrn_reflns_theta_min         2.470
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       Block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0299
_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)+(0.0079P)²+4.8157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6018
_reflns_number_total             6803
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02778b2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7705453--7705458.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7705453
_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   0.486
_shelx_estimated_absorpt_t_max   0.817
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
Dy Dy 0.51387(2) 0.61111(2) 0.57908(2) 0.02926(4) Uani 1 1 d . . . . .
Cl1 Cl 0.42924(7) 0.70505(6) -0.03452(6) 0.04232(18) Uani 1 1 d . . . . .
O1 O 0.49288(17) 0.54335(13) 0.40843(16) 0.0312(4) Uani 1 1 d . . . . .
O2 O 0.48331(19) 0.73851(14) 0.66853(18) 0.0375(5) Uani 1 1 d . . . . .
O3 O 0.56789(19) 0.72551(15) 0.48394(19) 0.0398(5) Uani 1 1 d . . . . .
O4 O 0.61573(18) 0.59062(15) 0.76528(18) 0.0384(5) Uani 1 1 d . . . . .
O5 O 0.70413(19) 0.59017(18) 0.5812(2) 0.0471(6) Uani 1 1 d . . . . .
N1 N 0.32537(19) 0.66309(17) 0.4402(2) 0.0309(5) Uani 1 1 d . . . . .
N2 N 0.6313(2) 0.42203(18) 0.3076(2) 0.0347(5) Uani 1 1 d . . . . .
C1 C 0.4796(2) 0.58515(19) 0.3117(2) 0.0295(6) Uani 1 1 d . . . . .
C2 C 0.3890(2) 0.64385(19) 0.2698(2) 0.0290(5) Uani 1 1 d . . . . .
C3 C 0.3733(2) 0.68041(19) 0.1626(2) 0.0303(6) Uani 1 1 d . . . . .
H3 H 0.310435 0.718003 0.132557 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4494(3) 0.6616(2) 0.1006(2) 0.0329(6) Uani 1 1 d . . . . .
C5 C 0.5420(3) 0.6081(2) 0.1437(3) 0.0361(6) Uani 1 1 d . . . . .
H5 H 0.594827 0.597368 0.101122 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5587(3) 0.5698(2) 0.2485(3) 0.0338(6) Uani 1 1 d . . . . .
C7 C 0.3101(2) 0.6704(2) 0.3341(2) 0.0309(6) Uani 1 1 d . . . . .
H7 H 0.240138 0.695581 0.292726 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2351(2) 0.7022(2) 0.4833(3) 0.0350(6) Uani 1 1 d . . . . .
H8A H 0.170612 0.719053 0.418916 0.042 Uiso 1 1 calc R U . . .
H8B H 0.264827 0.756086 0.525405 0.042 Uiso 1 1 calc R U . . .
C9 C 0.6610(3) 0.5143(2) 0.2992(3) 0.0395(7) Uani 1 1 d . . . . .
H9A H 0.715236 0.519050 0.252746 0.047 Uiso 1 1 calc R U . . .
H9B H 0.699352 0.536678 0.375202 0.047 Uiso 1 1 calc R U . . .
C10 C 0.7326(3) 0.3654(2) 0.3204(3) 0.0405(7) Uani 1 1 d . . . . .
H10A H 0.778256 0.388231 0.271563 0.049 Uiso 1 1 calc R U . . .
H10B H 0.706675 0.305950 0.293743 0.049 Uiso 1 1 calc R U . . .
C11 C 0.8086(3) 0.3590(2) 0.4400(3) 0.0403(7) Uani 1 1 d . . . . .
H11A H 0.817683 0.418149 0.473649 0.048 Uiso 1 1 calc R U . . .
H11B H 0.884812 0.338688 0.437256 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4895(3) 0.8193(2) 0.6512(3) 0.0348(6) Uani 1 1 d . . . . .
C13 C 0.5286(3) 0.8557(2) 0.5655(3) 0.0459(8) Uani 1 1 d . . . . .
H13 H 0.530484 0.917581 0.560072 0.055 Uiso 1 1 calc R U . . .
C14 C 0.5656(3) 0.8061(2) 0.4865(3) 0.0376(7) Uani 1 1 d . . . . .
C15 C 0.4507(4) 0.8784(2) 0.7317(3) 0.0537(9) Uani 1 1 d . . . . .
H15A H 0.372624 0.863157 0.731421 0.081 Uiso 1 1 calc R U . . .
H15B H 0.453214 0.939348 0.708224 0.081 Uiso 1 1 calc R U . . .
H15C H 0.501115 0.870870 0.807627 0.081 Uiso 1 1 calc R U . . .
C16 C 0.6079(3) 0.8513(3) 0.3964(3) 0.0535(9) Uani 1 1 d . . . . .
H16A H 0.690109 0.842214 0.411228 0.080 Uiso 1 1 calc R U . . .
H16B H 0.591911 0.914050 0.397018 0.080 Uiso 1 1 calc R U . . .
H16C H 0.569004 0.826879 0.322756 0.080 Uiso 1 1 calc R U . . .
C17 C 0.7155(3) 0.5704(2) 0.8159(3) 0.0361(6) Uani 1 1 d . . . . .
C18 C 0.8066(3) 0.5664(3) 0.7692(3) 0.0448(8) Uani 1 1 d . . . . .
H18 H 0.880033 0.554597 0.817443 0.054 Uiso 1 1 calc R U . . .
C19 C 0.7961(3) 0.5791(2) 0.6542(3) 0.0360(6) Uani 1 1 d . . . . .
C20 C 0.7350(3) 0.5490(3) 0.9394(3) 0.0471(8) Uani 1 1 d . . . . .
H20A H 0.701895 0.595221 0.975656 0.071 Uiso 1 1 calc R U . . .
H20B H 0.816872 0.545016 0.975422 0.071 Uiso 1 1 calc R U . . .
H20C H 0.698687 0.493077 0.947096 0.071 Uiso 1 1 calc R U . . .
C21 C 0.9033(3) 0.5801(3) 0.6132(3) 0.0446(8) Uani 1 1 d . . . . .
H21A H 0.924802 0.520055 0.600621 0.067 Uiso 1 1 calc R U . . .
H21B H 0.965396 0.607992 0.669980 0.067 Uiso 1 1 calc R U . . .
H21C H 0.888606 0.613063 0.542747 0.067 Uiso 1 1 calc R U . . .
H2N H 0.584(3) 0.412(3) 0.233(3) 0.054 Uiso 1 1 d . 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'
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'
Dy Dy -0.1892 4.4098 '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 Dy O3 81.40(7) . . ?
O1 Dy O2 145.36(7) . . ?
O3 Dy O2 73.15(8) . . ?
O1 Dy O4 138.13(7) . . ?
O3 Dy O4 117.29(8) . . ?
O2 Dy O4 75.69(8) . . ?
O1 Dy O5 79.18(8) . . ?
O3 Dy O5 71.87(9) . . ?
O2 Dy O5 113.40(9) . . ?
O4 Dy O5 72.96(8) . . ?
O1 Dy O1 67.27(8) . 3_666 ?
O3 Dy O1 144.17(7) . 3_666 ?
O2 Dy O1 142.49(7) . 3_666 ?
O4 Dy O1 79.61(8) . 3_666 ?
O5 Dy O1 85.10(8) . 3_666 ?
O1 Dy N2 119.01(8) . 3_666 ?
O3 Dy N2 139.27(8) . 3_666 ?
O2 Dy N2 71.63(8) . 3_666 ?
O4 Dy N2 72.44(8) . 3_666 ?
O5 Dy N2 142.24(8) . 3_666 ?
O1 Dy N2 74.25(7) 3_666 3_666 ?
O1 Dy N1 70.90(7) . . ?
O3 Dy N1 75.77(8) . . ?
O2 Dy N1 80.20(8) . . ?
O4 Dy N1 146.92(7) . . ?
O5 Dy N1 138.55(8) . . ?
O1 Dy N1 107.96(8) 3_666 . ?
N2 Dy N1 78.70(8) 3_666 . ?
O1 Dy Dy 34.20(5) . 3_666 ?
O3 Dy Dy 113.93(6) . 3_666 ?
O2 Dy Dy 165.96(6) . 3_666 ?
O4 Dy Dy 109.31(6) . 3_666 ?
O5 Dy Dy 80.61(7) . 3_666 ?
O1 Dy Dy 33.07(5) 3_666 3_666 ?
N2 Dy Dy 96.98(6) 3_666 3_666 ?
N1 Dy Dy 89.68(6) . 3_666 ?
C1 O1 Dy 124.42(18) . . ?
C1 O1 Dy 122.76(17) . 3_666 ?
Dy O1 Dy 112.73(8) . 3_666 ?
C12 O2 Dy 135.89(19) . . ?
C14 O3 Dy 137.3(2) . . ?
C17 O4 Dy 135.90(19) . . ?
C19 O5 Dy 136.3(2) . . ?
C7 N1 C8 114.8(2) . . ?
C7 N1 Dy 124.23(18) . . ?
C8 N1 Dy 120.06(18) . . ?
C9 N2 C10 110.8(2) . . ?
C9 N2 Dy 116.40(17) . 3_666 ?
C10 N2 Dy 120.04(18) . 3_666 ?
C9 N2 H2N 101(2) . . ?
C10 N2 H2N 106(2) . . ?
Dy N2 H2N 100(2) 3_666 . ?
O1 C1 C2 122.0(2) . . ?
O1 C1 C6 118.9(3) . . ?
C2 C1 C6 119.1(3) . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 C7 117.4(3) . . ?
C1 C2 C7 123.0(2) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.8(3) . . ?
C5 C4 Cl1 118.8(2) . . ?
C3 C4 Cl1 120.4(2) . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C9 121.7(3) . . ?
C1 C6 C9 118.5(3) . . ?
N1 C7 C2 126.7(3) . . ?
N1 C7 H7 116.6 . . ?
C2 C7 H7 116.6 . . ?
N1 C8 C11 113.3(3) . 3_666 ?
N1 C8 H8A 108.9 . . ?
C11 C8 H8A 108.9 3_666 . ?
N1 C8 H8B 108.9 . . ?
C11 C8 H8B 108.9 3_666 . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C6 112.4(3) . . ?
N2 C9 H9A 109.1 . . ?
C6 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
C6 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C11 114.4(3) . . ?
N2 C10 H10A 108.7 . . ?
C11 C10 H10A 108.7 . . ?
N2 C10 H10B 108.7 . . ?
C11 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C8 114.8(3) . 3_666 ?
C10 C11 H11A 108.6 . . ?
C8 C11 H11A 108.6 3_666 . ?
C10 C11 H11B 108.6 . . ?
C8 C11 H11B 108.6 3_666 . ?
H11A C11 H11B 107.5 . . ?
O2 C12 C13 124.8(3) . . ?
O2 C12 C15 115.5(3) . . ?
C13 C12 C15 119.7(3) . . ?
C12 C13 C14 123.7(3) . . ?
C12 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
O3 C14 C13 124.9(3) . . ?
O3 C14 C16 115.0(3) . . ?
C13 C14 C16 120.1(3) . . ?
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 125.9(3) . . ?
O4 C17 C20 115.1(3) . . ?
C18 C17 C20 119.0(3) . . ?
C17 C18 C19 123.4(3) . . ?
C17 C18 H18 118.3 . . ?
C19 C18 H18 118.3 . . ?
O5 C19 C18 124.7(3) . . ?
O5 C19 C21 116.3(3) . . ?
C18 C19 C21 119.0(3) . . ?
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
Dy O1 2.3020(19) . ?
Dy O3 2.302(2) . ?
Dy O2 2.321(2) . ?
Dy O4 2.323(2) . ?
Dy O5 2.337(2) . ?
Dy O1 2.371(2) 3_666 ?
Dy N2 2.588(2) 3_666 ?
Dy N1 2.595(2) . ?
Dy Dy 3.8909(4) 3_666 ?
Cl1 C4 1.753(3) . ?
O1 C1 1.327(3) . ?
O2 C12 1.261(4) . ?
O3 C14 1.234(4) . ?
O4 C17 1.248(4) . ?
O5 C19 1.247(4) . ?
N1 C7 1.279(4) . ?
N1 C8 1.474(3) . ?
N2 C9 1.468(4) . ?
N2 C10 1.482(4) . ?
N2 H2N 0.95(4) . ?
C1 C2 1.410(4) . ?
C1 C6 1.415(4) . ?
C2 C3 1.403(4) . ?
C2 C7 1.462(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(5) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 C9 1.500(4) . ?
C7 H7 0.9500 . ?
C8 C11 1.527(4) 3_666 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.391(4) . ?
C12 C15 1.512(4) . ?
C13 C14 1.403(5) . ?
C13 H13 0.9500 . ?
C14 C16 1.515(4) . ?
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 1.386(4) . ?
C17 C20 1.517(4) . ?
C18 C19 1.406(5) . ?
C18 H18 0.9500 . ?
C19 C21 1.526(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
