#------------------------------------------------------------------------------
#$Date: 2020-07-06 05:53:38 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/46/7704613.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_7704613
loop_
_publ_author_name
'Fondo, Matilde'
'Corredoira-Vázquez, Julio'
'García-Deibe, Ana M'
'Gómez-Coca, Silvia'
'Ruiz, Eliseo'
'Sanmartín-Matalobos, Jesús'
_publ_section_title
;
 Dysprosium-based complexes with a flat pentadentate donor: a magnetic and
 ab initio study.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8389
_journal_page_last               8401
_journal_paper_doi               10.1039/d0dt01293a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H26 Dy N4 O6, C19 H13 Cl2 Dy N3 O2'
_chemical_formula_sum            'C47 H39 Cl2 Dy2 N7 O8'
_chemical_formula_weight         1225.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.517(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.188(4)
_cell_length_b                   18.419(4)
_cell_length_c                   12.866(3)
_cell_measurement_reflns_used    2900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.275
_cell_measurement_theta_min      3.1
_cell_volume                     4439.1(17)
_computing_cell_refinement       'BRUKER APEX3'
_computing_data_collection       'BRUKER APEX3'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'WinGX 2020.1 (Farrugia, 2012)'
_computing_publication_material  'WinGX 2020.1 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13092
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.390
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.525
_exptl_absorpt_correction_T_max  0.959344
_exptl_absorpt_correction_T_min  0.337817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012.1 (Bruker AXS,2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.352
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0761
_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)+(0.1074P)²+43.6418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4622
_reflns_number_total             6438
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01293a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7704612--7704615.cif.'
_cod_original_cell_volume        4439.2(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7704613
_shelx_shelxl_version_number     2018/1
_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   0.620
_shelx_estimated_absorpt_t_max   0.872
_exptl_absorpt_special_details
;
4 twin components present. Reflections merged according to point-group 2/m   
 Single reflections that also occur in composites omitted
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Dy1 Dy 0.500000 0.91946(5) 0.750000 0.0338(3) Uani 1 2 d S T P . .
O11 O 0.5839(5) 1.0007(5) 0.8133(6) 0.040(2) Uani 1 1 d . . . . .
N11 N 0.5684(7) 0.9542(7) 0.6175(8) 0.046(3) Uani 1 1 d . . . . .
N12 N 0.4591(7) 0.8635(6) 0.5711(7) 0.045(3) Uani 1 1 d . . . . .
C101 C 0.6318(8) 1.0211(8) 0.7628(10) 0.044(3) Uani 1 1 d . . . . .
C102 C 0.6910(9) 1.0659(10) 0.8075(12) 0.063(5) Uani 1 1 d . . . . .
H102 H 0.697836 1.079315 0.880278 0.075 Uiso 1 1 calc R U . . .
C103 C 0.7378(9) 1.0901(14) 0.7514(15) 0.079(6) Uani 1 1 d . . . . .
H103 H 0.775227 1.122396 0.782049 0.094 Uiso 1 1 calc R U . . .
C104 C 0.7286(12) 1.0644(14) 0.6384(16) 0.089(7) Uani 1 1 d . . . . .
H104 H 0.762330 1.078460 0.597891 0.106 Uiso 1 1 calc R U . . .
C105 C 0.6753(9) 1.0231(11) 0.5954(14) 0.065(5) Uani 1 1 d . . . . .
H105 H 0.669638 1.009258 0.522913 0.077 Uiso 1 1 calc R U . . .
C106 C 0.6264(8) 0.9988(9) 0.6524(10) 0.049(4) Uani 1 1 d . . . . .
C107 C 0.5530(10) 0.9305(8) 0.5202(10) 0.055(4) Uani 1 1 d . . . . .
H107 H 0.579559 0.945122 0.469519 0.066 Uiso 1 1 calc R U . . .
C108 C 0.4931(9) 0.8807(8) 0.4926(9) 0.048(4) Uani 1 1 d . U . . .
C109 C 0.4686(13) 0.8542(10) 0.3896(10) 0.075(7) Uani 1 1 d . U . . .
H109 H 0.491778 0.867004 0.334015 0.089 Uiso 1 1 calc R U . . .
C110 C 0.4092(12) 0.8086(9) 0.3699(11) 0.071(6) Uani 1 1 d . . . . .
H110 H 0.391827 0.790214 0.300130 0.085 Uiso 1 1 calc R U . . .
C111 C 0.3762(12) 0.7902(8) 0.4478(11) 0.063(5) Uani 1 1 d . . . . .
H111 H 0.336196 0.758582 0.435227 0.076 Uiso 1 1 calc R U . . .
C112 C 0.4043(9) 0.8207(8) 0.5514(9) 0.049(4) Uani 1 1 d . . . . .
C113 C 0.3664(8) 0.8049(9) 0.6396(11) 0.051(4) Uani 1 1 d . . . . .
H113 H 0.351916 0.752715 0.638658 0.061 Uiso 1 1 calc R U . . .
C114 C 0.2665(9) 0.8439(14) 0.6998(18) 0.082(6) Uani 1 1 d . . . . .
H11A H 0.258923 0.792428 0.712973 0.124 Uiso 1 1 calc R U . . .
H11B H 0.220322 0.867789 0.674543 0.124 Uiso 1 1 calc R U . . .
H11C H 0.291652 0.866995 0.766042 0.124 Uiso 1 1 calc R U . . .
Dy2 Dy 0.500000 0.62161(5) 0.750000 0.0356(3) Uani 1 2 d S T P . .
Cl2 Cl 0.39427(19) 0.61762(19) 0.5834(3) 0.0430(8) Uani 1 1 d . . . . .
N21 N 0.4329(6) 0.5640(6) 0.8750(8) 0.036(2) Uani 1 1 d . . . . .
N22 N 0.500000 0.4869(8) 0.750000 0.037(3) Uani 1 2 d S T P . .
O12 O 0.4139(5) 0.8230(5) 0.7382(6) 0.042(2) Uani 1 1 d . . . . .
H12 H 0.422441 0.791154 0.765833 0.051 Uiso 1 1 d R U . . .
O21 O 0.4416(5) 0.7038(5) 0.8340(7) 0.040(2) Uani 1 1 d . . . . .
O13 O 0.3068(7) 0.8503(8) 0.6241(9) 0.073(4) Uani 1 1 d . . . . .
C201 C 0.4092(7) 0.6869(7) 0.9096(8) 0.031(3) Uani 1 1 d . . . . .
C202 C 0.3768(7) 0.7374(8) 0.9641(11) 0.041(3) Uani 1 1 d . . . . .
H202 H 0.380417 0.787435 0.948324 0.050 Uiso 1 1 calc R U . . .
C203 C 0.3389(8) 0.7173(9) 1.0414(11) 0.052(4) Uani 1 1 d . . . . .
H203 H 0.317086 0.753253 1.076762 0.062 Uiso 1 1 calc R U . . .
C204 C 0.3337(7) 0.6437(9) 1.0658(10) 0.044(3) Uani 1 1 d . . . . .
H204 H 0.309703 0.629580 1.119797 0.053 Uiso 1 1 calc R U . . .
C205 C 0.3633(8) 0.5920(8) 1.0117(10) 0.043(3) Uani 1 1 d . . . . .
H205 H 0.358400 0.541887 1.026342 0.052 Uiso 1 1 calc R U . . .
C206 C 0.4006(7) 0.6135(7) 0.9351(10) 0.036(3) Uani 1 1 d . . . . .
C207 C 0.4312(8) 0.4955(8) 0.8855(11) 0.042(3) Uani 1 1 d . . . . .
H207 H 0.408607 0.473795 0.936609 0.050 Uiso 1 1 calc R U . . .
C208 C 0.4658(7) 0.4505(7) 0.8151(10) 0.041(3) Uani 1 1 d . . . . .
C209 C 0.4671(8) 0.3751(8) 0.8165(13) 0.050(4) Uani 1 1 d . . . . .
H209 H 0.444678 0.350063 0.864858 0.060 Uiso 1 1 calc R U . . .
C210 C 0.500000 0.3354(11) 0.750000 0.042(4) Uani 1 2 d S T P . .
H210 H 0.500001 0.283857 0.749998 0.051 Uiso 1 2 calc R U P . .
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
O11 Dy1 O11 95.2(5) . 2_656 ?
O11 Dy1 O12 162.5(3) . . ?
O11 Dy1 O12 92.4(3) 2_656 . ?
O11 Dy1 O12 92.4(3) . 2_656 ?
O11 Dy1 O12 162.5(3) 2_656 2_656 ?
O12 Dy1 O12 84.9(5) . 2_656 ?
O11 Dy1 N11 91.4(3) . 2_656 ?
O11 Dy1 N11 67.9(4) 2_656 2_656 ?
O12 Dy1 N11 76.9(3) . 2_656 ?
O12 Dy1 N11 127.7(4) 2_656 2_656 ?
O11 Dy1 N11 67.9(4) . . ?
O11 Dy1 N11 91.4(3) 2_656 . ?
O12 Dy1 N11 127.7(4) . . ?
O12 Dy1 N11 76.9(3) 2_656 . ?
N11 Dy1 N11 149.7(6) 2_656 . ?
O11 Dy1 N12 83.2(3) . 2_656 ?
O11 Dy1 N12 132.6(4) 2_656 2_656 ?
O12 Dy1 N12 80.0(3) . 2_656 ?
O12 Dy1 N12 64.0(3) 2_656 2_656 ?
N11 Dy1 N12 64.8(5) 2_656 2_656 ?
N11 Dy1 N12 130.0(4) . 2_656 ?
O11 Dy1 N12 132.6(4) . . ?
O11 Dy1 N12 83.2(3) 2_656 . ?
O12 Dy1 N12 64.0(3) . . ?
O12 Dy1 N12 80.0(3) 2_656 . ?
N11 Dy1 N12 130.0(4) 2_656 . ?
N11 Dy1 N12 64.8(5) . . ?
N12 Dy1 N12 131.1(5) 2_656 . ?
C101 O11 Dy1 123.4(9) . . ?
C107 N11 C106 120.9(13) . . ?
C107 N11 Dy1 122.6(12) . . ?
C106 N11 Dy1 116.4(8) . . ?
C112 N12 C108 119.9(12) . . ?
C112 N12 Dy1 120.9(9) . . ?
C108 N12 Dy1 119.2(10) . . ?
O11 C101 C102 124.0(13) . . ?
O11 C101 C106 119.9(14) . . ?
C102 C101 C106 116.1(14) . . ?
C103 C102 C101 122.9(17) . . ?
C102 C103 C104 117.6(19) . . ?
C105 C104 C103 120.8(17) . . ?
C104 C105 C106 121.7(18) . . ?
N11 C106 C105 127.8(14) . . ?
N11 C106 C101 111.5(12) . . ?
C105 C106 C101 120.7(16) . . ?
N11 C107 C108 116.8(13) . . ?
N12 C108 C109 120.6(18) . . ?
N12 C108 C107 116.6(11) . . ?
C109 C108 C107 122.7(15) . . ?
C110 C109 C108 118.5(16) . . ?
C111 C110 C109 121.1(14) . . ?
C110 C111 C112 116.9(18) . . ?
N12 C112 C111 123.0(15) . . ?
N12 C112 C113 118.4(12) . . ?
C111 C112 C113 118.6(16) . . ?
O13 C113 O12 109.3(12) . . ?
O13 C113 C112 107.0(13) . . ?
O12 C113 C112 107.8(12) . . ?
O21 Dy2 O21 97.2(5) . 2_656 ?
O21 Dy2 N22 131.4(2) . . ?
O21 Dy2 N22 131.4(2) 2_656 . ?
O21 Dy2 N21 163.0(3) . 2_656 ?
O21 Dy2 N21 66.7(3) 2_656 2_656 ?
N22 Dy2 N21 64.9(3) . 2_656 ?
O21 Dy2 N21 66.7(3) . . ?
O21 Dy2 N21 163.0(3) 2_656 . ?
N22 Dy2 N21 64.9(3) . . ?
N21 Dy2 N21 129.8(5) 2_656 . ?
O21 Dy2 Cl2 91.9(2) . . ?
O21 Dy2 Cl2 90.2(2) 2_656 . ?
N22 Dy2 Cl2 88.39(8) . . ?
N21 Dy2 Cl2 82.9(3) 2_656 . ?
N21 Dy2 Cl2 95.7(3) . . ?
O21 Dy2 Cl2 90.2(2) . 2_656 ?
O21 Dy2 Cl2 91.9(2) 2_656 2_656 ?
N22 Dy2 Cl2 88.39(8) . 2_656 ?
N21 Dy2 Cl2 95.7(3) 2_656 2_656 ?
N21 Dy2 Cl2 82.9(3) . 2_656 ?
Cl2 Dy2 Cl2 176.77(16) . 2_656 ?
C207 N21 C206 123.7(11) . . ?
C207 N21 Dy2 121.2(9) . . ?
C206 N21 Dy2 115.0(8) . . ?
C208 N22 C208 120.4(17) 2_656 . ?
C208 N22 Dy2 119.8(8) 2_656 . ?
C208 N22 Dy2 119.8(8) . . ?
C113 O12 Dy1 121.6(9) . . ?
C201 O21 Dy2 123.9(8) . . ?
C114 O13 C113 114.6(15) . . ?
O21 C201 C202 123.8(12) . . ?
O21 C201 C206 120.1(11) . . ?
C202 C201 C206 115.9(11) . . ?
C201 C202 C203 122.7(14) . . ?
C204 C203 C202 119.1(14) . . ?
C205 C204 C203 120.1(12) . . ?
C204 C205 C206 119.4(13) . . ?
C205 C206 C201 122.8(12) . . ?
C205 C206 N21 123.5(12) . . ?
C201 C206 N21 113.7(10) . . ?
N21 C207 C208 117.6(12) . . ?
N22 C208 C209 119.6(14) . . ?
N22 C208 C207 116.3(12) . . ?
C209 C208 C207 124.0(13) . . ?
C210 C209 C208 122.2(14) . . ?
C209 C210 C209 115.9(18) 2_656 . ?
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
Dy1 O11 2.218(9) . ?
Dy1 O11 2.218(9) 2_656 ?
Dy1 O12 2.409(10) . ?
Dy1 O12 2.409(9) 2_656 ?
Dy1 N11 2.451(11) 2_656 ?
Dy1 N11 2.451(11) . ?
Dy1 N12 2.488(10) 2_656 ?
Dy1 N12 2.488(10) . ?
O11 C101 1.293(16) . ?
N11 C107 1.297(17) . ?
N11 C106 1.38(2) . ?
N12 C112 1.30(2) . ?
N12 C108 1.353(18) . ?
C101 C102 1.42(2) . ?
C101 C106 1.459(18) . ?
C102 C103 1.34(2) . ?
C103 C104 1.50(3) . ?
C104 C105 1.30(3) . ?
C105 C106 1.38(2) . ?
C107 C108 1.45(2) . ?
C108 C109 1.396(19) . ?
C109 C110 1.39(3) . ?
C110 C111 1.34(3) . ?
C111 C112 1.439(18) . ?
C112 C113 1.50(2) . ?
C113 O13 1.40(2) . ?
C113 O12 1.431(15) . ?
C114 O13 1.37(2) . ?
Dy2 O21 2.289(9) . ?
Dy2 O21 2.289(9) 2_656 ?
Dy2 N22 2.482(15) . ?
Dy2 N21 2.504(10) 2_656 ?
Dy2 N21 2.504(10) . ?
Dy2 Cl2 2.613(3) . ?
Dy2 Cl2 2.613(3) 2_656 ?
N21 C207 1.269(17) . ?
N21 C206 1.422(16) . ?
N22 C208 1.348(15) 2_656 ?
N22 C208 1.349(15) . ?
O21 C201 1.300(14) . ?
C201 C202 1.389(17) . ?
C201 C206 1.410(18) . ?
C202 C203 1.40(2) . ?
C203 C204 1.40(2) . ?
C204 C205 1.374(19) . ?
C205 C206 1.395(17) . ?
C207 C208 1.49(2) . ?
C208 C209 1.390(19) . ?
C209 C210 1.377(19) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C107 H107 O11 0.95 2.26 3.120(16) 149.7 6_575 yes
C113 H113 Cl2 1.00 2.76 3.588(17) 140.6 . yes
O12 H12 O21 0.69 1.83 2.518(13) 176.9 . yes
C207 H207 Cl2 0.95 2.59 3.479(13) 156.2 6_566 yes
