#------------------------------------------------------------------------------
#$Date: 2021-11-19 02:04:31 +0200 (Fri, 19 Nov 2021) $
#$Revision: 270757 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708886.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_7708886
loop_
_publ_author_name
'Dong, Yubao'
'Zhu, Li'
'Yin, Bing'
'Zhu, Xinrui'
'Li, Dongfeng'
_publ_section_title
;
 Regulating the magnetic properties of seven-coordinated Dy(III)
 single-ion magnets through the effect of positional isomers on axial
 crystal-field.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d1dt02925h
_journal_year                    2021
_chemical_formula_moiety         'C30 H32 Cl Dy N4 O4'
_chemical_formula_sum            'C30 H32 Cl Dy N4 O4'
_chemical_formula_weight         710.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.04.09 svn.r3586 for OlexSys, GUI svn.r5731)
;
_audit_update_record
;
2021-03-19 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6217(12)
_cell_length_b                   17.052(2)
_cell_length_c                   19.783(3)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.39
_cell_volume                     2908.4(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24106
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_min         2.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.6328.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00067(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0279
_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)+4.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2658
_reflns_number_total             3528
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02925h2.cif
_cod_data_source_block           mo_200803f_0m
_cod_original_cell_volume        2908.5(7)
_cod_database_code               7708886
_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_max   0.774
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C12(H12), C13(H13)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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 0.000000 0.28204(2) 0.250000 0.03449(8) Uani 1 2 d S T P . .
Cl1 Cl 0.000000 0.12581(6) 0.250000 0.0506(3) Uani 1 2 d S T P . .
O1 O 0.1139(3) 0.30687(13) 0.34514(12) 0.0455(6) Uani 1 1 d . . . . .
O2 O 0.3175(5) 0.57316(19) 0.47791(15) 0.0859(11) Uani 1 1 d . . . . .
N1 N 0.2484(4) 0.25724(16) 0.17993(16) 0.0472(7) Uani 1 1 d . . . . .
N2 N 0.1589(3) 0.40606(14) 0.22226(14) 0.0352(6) Uani 1 1 d . . . . .
C1 C 0.3236(5) 0.1885(2) 0.1746(2) 0.0633(12) Uani 1 1 d . . . . .
H1 H 0.281762 0.144969 0.196234 0.076 Uiso 1 1 calc R . . . .
C2 C 0.4591(5) 0.1792(2) 0.1388(3) 0.0671(13) Uani 1 1 d . . . . .
H2 H 0.507250 0.130499 0.136411 0.081 Uiso 1 1 calc R . . . .
C3 C 0.5219(5) 0.2428(2) 0.1070(2) 0.0591(11) Uani 1 1 d . . . . .
H3 H 0.613948 0.238221 0.082786 0.071 Uiso 1 1 calc R . . . .
C4 C 0.4461(5) 0.3141(2) 0.11132(18) 0.0464(8) Uani 1 1 d . . . . .
H4 H 0.486018 0.358119 0.089692 0.056 Uiso 1 1 calc R . . . .
C5 C 0.3107(4) 0.31909(19) 0.14810(17) 0.0401(7) Uani 1 1 d . . . . .
C6 C 0.2244(4) 0.39559(19) 0.15363(17) 0.0417(8) Uani 1 1 d . . . . .
H6A H 0.294388 0.438590 0.143647 0.050 Uiso 1 1 calc R . . . .
H6B H 0.141151 0.396638 0.120653 0.050 Uiso 1 1 calc R . . . .
C7 C 0.0621(4) 0.47800(17) 0.22254(19) 0.0414(8) Uani 1 1 d . . . . .
H7A H 0.012282 0.483353 0.178828 0.050 Uiso 1 1 calc R . . . .
H7B H 0.128866 0.523196 0.228935 0.050 Uiso 1 1 calc R . . . .
C8 C 0.2933(4) 0.4140(2) 0.26991(17) 0.0404(8) Uani 1 1 d . . . . .
H8A H 0.357176 0.457456 0.254915 0.048 Uiso 1 1 calc R . . . .
H8B H 0.355779 0.366798 0.266844 0.048 Uiso 1 1 calc R . . . .
C9 C 0.2519(4) 0.4270(2) 0.34269(17) 0.0402(7) Uani 1 1 d . . . . .
C10 C 0.3044(4) 0.4951(2) 0.37499(18) 0.0459(8) Uani 1 1 d . . . . .
H10 H 0.360244 0.532396 0.350817 0.055 Uiso 1 1 calc R . . . .
C11 C 0.2734(5) 0.5069(2) 0.4426(2) 0.0566(10) Uani 1 1 d . . . . .
C12 C 0.1912(6) 0.4500(2) 0.4781(2) 0.0622(11) Uani 1 1 d . . . . .
H12 H 0.170961 0.457360 0.523829 0.075 Uiso 1 1 calc R . . . .
C13 C 0.1392(5) 0.3827(2) 0.44625(19) 0.0536(10) Uani 1 1 d . . . . .
H13 H 0.084513 0.345399 0.470902 0.064 Uiso 1 1 calc R . . . .
C14 C 0.1677(4) 0.3700(2) 0.37762(18) 0.0421(8) Uani 1 1 d . . . . .
C15 C 0.4072(8) 0.6286(3) 0.4424(2) 0.0934(19) Uani 1 1 d . . . . .
H15A H 0.351653 0.645616 0.403004 0.140 Uiso 1 1 calc GR . . . .
H15B H 0.503662 0.605187 0.429011 0.140 Uiso 1 1 calc GR . . . .
H15C H 0.427459 0.672898 0.471084 0.140 Uiso 1 1 calc GR . . . .
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'
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'
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
_geom_angle_publ_flag
O1 Dy1 Cl1 101.28(6) . . ?
O1 Dy1 Cl1 101.28(6) 3 . ?
O1 Dy1 O1 157.44(12) 3 . ?
O1 Dy1 N1 86.64(10) . 3 ?
O1 Dy1 N1 86.64(10) 3 . ?
O1 Dy1 N1 97.04(10) . . ?
O1 Dy1 N1 97.04(10) 3 3 ?
O1 Dy1 N2 84.00(9) 3 . ?
O1 Dy1 N2 77.51(9) 3 3 ?
O1 Dy1 N2 77.51(9) . . ?
O1 Dy1 N2 84.00(9) . 3 ?
N1 Dy1 Cl1 80.59(6) . . ?
N1 Dy1 Cl1 80.59(6) 3 . ?
N1 Dy1 N1 161.17(13) . 3 ?
N2 Dy1 Cl1 145.08(6) 3 . ?
N2 Dy1 Cl1 145.08(6) . . ?
N2 Dy1 N1 65.17(9) . . ?
N2 Dy1 N1 65.16(9) 3 3 ?
N2 Dy1 N1 133.49(9) 3 . ?
N2 Dy1 N1 133.49(9) . 3 ?
N2 Dy1 N2 69.83(12) 3 . ?
C14 O1 Dy1 137.1(2) . . ?
C11 O2 C15 116.7(3) . . ?
C1 N1 Dy1 125.8(3) . . ?
C5 N1 Dy1 117.1(2) . . ?
C5 N1 C1 117.1(3) . . ?
C6 N2 Dy1 107.37(18) . . ?
C6 N2 C7 108.5(3) . . ?
C6 N2 C8 107.0(3) . . ?
C7 N2 Dy1 112.22(19) . . ?
C7 N2 C8 111.0(3) . . ?
C8 N2 Dy1 110.51(18) . . ?
N1 C1 C2 123.4(4) . . ?
C3 C2 C1 118.9(4) . . ?
C2 C3 C4 118.8(4) . . ?
C5 C4 C3 119.2(4) . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 116.7(3) . . ?
C4 C5 C6 120.7(3) . . ?
N2 C6 C5 111.1(3) . . ?
N2 C7 C7 113.4(2) . 3 ?
N2 C8 C9 115.7(3) . . ?
C10 C9 C8 119.0(3) . . ?
C14 C9 C8 119.7(3) . . ?
C14 C9 C10 121.3(3) . . ?
C11 C10 C9 120.0(4) . . ?
O2 C11 C12 117.1(4) . . ?
C10 C11 O2 123.8(4) . . ?
C10 C11 C12 119.1(4) . . ?
C13 C12 C11 120.9(4) . . ?
C12 C13 C14 120.9(4) . . ?
O1 C14 C9 120.2(3) . . ?
O1 C14 C13 122.1(3) . . ?
C9 C14 C13 117.7(3) . . ?
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 Cl1 2.6641(11) . ?
Dy1 O1 2.165(2) . ?
Dy1 O1 2.165(2) 3 ?
Dy1 N1 2.586(3) 3 ?
Dy1 N1 2.586(3) . ?
Dy1 N2 2.579(3) . ?
Dy1 N2 2.579(3) 3 ?
O1 C14 1.338(4) . ?
O2 C11 1.382(5) . ?
O2 C15 1.409(6) . ?
N1 C1 1.343(5) . ?
N1 C5 1.341(4) . ?
N2 C6 1.481(4) . ?
N2 C7 1.484(4) . ?
N2 C8 1.500(4) . ?
C1 C2 1.376(6) . ?
C2 C3 1.366(6) . ?
C3 C4 1.383(6) . ?
C4 C5 1.378(5) . ?
C5 C6 1.506(5) . ?
C7 C7 1.526(7) 3 ?
C8 C9 1.500(5) . ?
C9 C10 1.400(5) . ?
C9 C14 1.396(5) . ?
C10 C11 1.379(5) . ?
C11 C12 1.390(6) . ?
C12 C13 1.384(5) . ?
C13 C14 1.397(5) . ?
