#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:33:11 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/70/7707002.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_7707002
loop_
_publ_author_name
'Yang, Yan'
'Zhou, Zhen'
'Wei, Zu-Zhuang'
'Qin, Qi-Pin'
'Yang, Lin'
'Liang, Hong'
_publ_section_title
;
 High anticancer activity and apoptosis- and autophagy-inducing properties
 of novel lanthanide(III) complexes bearing
 8-hydroxyquinoline-N-oxide and 1,10-phenanthroline.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5828
_journal_page_last               5834
_journal_paper_doi               10.1039/d1dt00450f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C21 H16 Cl2 Dy N3 O3'
_chemical_formula_sum            'C21 H16 Cl2 Dy N3 O3'
_chemical_formula_weight         591.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-17
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.06 svn.r2239, GUI svn.r4109)
;
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2021-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8681(4)
_cell_length_b                   11.0471(4)
_cell_length_c                   18.2005(4)
_cell_measurement_reflns_used    3573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0290
_cell_measurement_theta_min      3.6690
_cell_volume                     1981.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.8848
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     21.00  61.00   1.00    1.50    --   18.78 -99.00   0.00   40
  2  ω    -86.00   9.00   1.00    1.50    --  -19.10 -77.00  90.00   95
  3  ω    -25.00   1.00   1.00    1.50    --  -19.10 -57.00-150.00   26
  4  ω    -48.00  48.00   1.00    1.50    --  -19.10  77.00-150.00   96
  5  ω    -54.00  43.00   1.00    1.50    --  -19.10  19.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0382444000
_diffrn_orient_matrix_UB_12      0.0540001000
_diffrn_orient_matrix_UB_13      0.0052508000
_diffrn_orient_matrix_UB_21      -0.0560699000
_diffrn_orient_matrix_UB_22      0.0343351000
_diffrn_orient_matrix_UB_23      -0.0143287000
_diffrn_orient_matrix_UB_31      -0.0238919000
_diffrn_orient_matrix_UB_32      0.0057263000
_diffrn_orient_matrix_UB_33      0.0359048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12454
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           n/a
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    4.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0338
_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)+(0.0298P)²+2.2449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3254
_reflns_number_total             4054
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00450f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7706997--7707003.cif.'
_cod_original_cell_volume        1981.36(11)
_cod_database_code               7707002
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.644
_oxdiff_exptl_absorpt_empirical_full_min 0.746
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.72897(2) 0.65153(2) 0.08400(2) 0.02807(10) Uani 1 1 d . . . . .
Cl1 Cl 0.99220(14) 0.64422(14) 0.05867(8) 0.0440(4) Uani 1 1 d . . . . .
Cl2 Cl 0.48412(14) 0.58590(13) 0.12347(7) 0.0392(3) Uani 1 1 d . . . . .
O1 O 0.7385(4) 0.4675(3) 0.01180(18) 0.0379(9) Uani 1 1 d . . . . .
H1A H 0.8159 0.4255 0.0023 0.057 Uiso 1 1 d R U . . .
H1B H 0.6652 0.4285 -0.0104 0.057 Uiso 1 1 d R U . . .
O2 O 0.6398(4) 0.6854(3) -0.02883(19) 0.0429(10) Uani 1 1 d . . . . .
O3 O 0.7212(4) 0.8462(3) 0.07112(19) 0.0377(9) Uani 1 1 d . . . . .
N1 N 0.7934(4) 0.4945(4) 0.1829(2) 0.0329(10) Uani 1 1 d . . . . .
N2 N 0.7903(4) 0.7370(4) 0.2124(2) 0.0333(10) Uani 1 1 d . . . . .
N3 N 0.6010(4) 0.7787(4) -0.0710(2) 0.0320(10) Uani 1 1 d . . . . .
C1 C 0.5393(5) 0.7489(6) -0.1357(3) 0.0395(13) Uani 1 1 d . . . . .
H1 H 0.5198 0.6683 -0.1465 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5041(6) 0.8392(6) -0.1870(3) 0.0448(15) Uani 1 1 d . . . . .
H2 H 0.4617 0.8187 -0.2321 0.054 Uiso 1 1 calc R U . . .
C3 C 0.5318(5) 0.9569(6) -0.1710(3) 0.0446(15) Uani 1 1 d . . . . .
H3 H 0.5092 1.0167 -0.2054 0.054 Uiso 1 1 calc R U . . .
C4 C 0.5946(5) 0.9888(5) -0.1026(3) 0.0374(13) Uani 1 1 d . . . . .
C5 C 0.6277(5) 0.8963(5) -0.0507(3) 0.0290(11) Uani 1 1 d . . . . .
C6 C 0.6916(5) 0.9268(5) 0.0197(3) 0.0319(12) Uani 1 1 d . . . . .
C7 C 0.7179(6) 1.0471(5) 0.0336(3) 0.0434(14) Uani 1 1 d . . . . .
H7 H 0.7577 1.0686 0.0792 0.052 Uiso 1 1 calc R U . . .
C8 C 0.6874(7) 1.1387(5) -0.0179(4) 0.0480(16) Uani 1 1 d . . . . .
H8 H 0.7098 1.2187 -0.0069 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6239(6) 1.1098(6) -0.0850(4) 0.0489(16) Uani 1 1 d . . . . .
H9 H 0.6006 1.1708 -0.1186 0.059 Uiso 1 1 calc R U . . .
C10 C 0.7859(6) 0.8527(5) 0.2311(3) 0.0396(14) Uani 1 1 d . . . . .
H10 H 0.7543 0.9064 0.1947 0.047 Uiso 1 1 calc R U . . .
C11 C 0.8228(6) 0.9014(6) 0.2978(3) 0.0443(15) Uani 1 1 d . . . . .
H11 H 0.8122 0.9837 0.3066 0.053 Uiso 1 1 calc R U . . .
C12 C 0.8757(6) 0.8266(6) 0.3513(3) 0.0452(15) Uani 1 1 d . . . . .
H12 H 0.9055 0.8575 0.3968 0.054 Uiso 1 1 calc R U . . .
C13 C 0.8846(5) 0.7034(6) 0.3370(3) 0.0385(13) Uani 1 1 d . . . . .
C14 C 0.9368(6) 0.6157(7) 0.3901(3) 0.0502(17) Uani 1 1 d . . . . .
H14 H 0.9703 0.6427 0.4360 0.060 Uiso 1 1 calc R U . . .
C15 C 0.9386(6) 0.4972(7) 0.3757(3) 0.0481(16) Uani 1 1 d . . . . .
H15 H 0.9736 0.4437 0.4113 0.058 Uiso 1 1 calc R U . . .
C16 C 0.8872(5) 0.4515(6) 0.3059(3) 0.0396(13) Uani 1 1 d . . . . .
C17 C 0.8733(6) 0.3279(6) 0.2917(3) 0.0452(15) Uani 1 1 d . . . . .
H17 H 0.8980 0.2716 0.3280 0.054 Uiso 1 1 calc R U . . .
C18 C 0.8233(6) 0.2906(6) 0.2245(3) 0.0442(14) Uani 1 1 d . . . . .
H18 H 0.8144 0.2086 0.2138 0.053 Uiso 1 1 calc R U . . .
C19 C 0.7858(6) 0.3771(5) 0.1721(3) 0.0395(13) Uani 1 1 d . . . . .
H19 H 0.7531 0.3501 0.1261 0.047 Uiso 1 1 calc R U . . .
C20 C 0.8405(5) 0.5327(5) 0.2510(2) 0.0300(11) Uani 1 1 d . . . . .
C21 C 0.8397(5) 0.6603(5) 0.2663(3) 0.0309(12) 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'
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
Cl2 Dy1 Cl1 161.35(5) . . ?
O1 Dy1 Cl1 79.32(9) . . ?
O1 Dy1 Cl2 88.83(9) . . ?
O1 Dy1 N1 78.32(12) . . ?
O1 Dy1 N2 142.06(13) . . ?
O2 Dy1 Cl1 100.81(12) . . ?
O2 Dy1 Cl2 88.52(11) . . ?
O2 Dy1 O1 70.45(13) . . ?
O2 Dy1 N1 146.78(14) . . ?
O2 Dy1 N2 147.49(14) . . ?
O3 Dy1 Cl1 92.33(11) . . ?
O3 Dy1 Cl2 105.84(11) . . ?
O3 Dy1 O1 140.94(12) . . ?
O3 Dy1 O2 73.90(13) . . ?
O3 Dy1 N1 139.16(14) . . ?
O3 Dy1 N2 74.81(13) . . ?
N1 Dy1 Cl1 83.84(10) . . ?
N1 Dy1 Cl2 79.65(10) . . ?
N1 Dy1 N2 64.51(14) . . ?
N2 Dy1 Cl1 89.03(10) . . ?
N2 Dy1 Cl2 91.64(10) . . ?
N3 O2 Dy1 138.7(3) . . ?
C6 O3 Dy1 139.1(3) . . ?
C19 N1 Dy1 123.6(3) . . ?
C19 N1 C20 117.1(4) . . ?
C20 N1 Dy1 119.3(3) . . ?
C10 N2 Dy1 125.5(4) . . ?
C10 N2 C21 115.4(5) . . ?
C21 N2 Dy1 119.0(3) . . ?
O2 N3 C1 114.9(4) . . ?
O2 N3 C5 122.3(4) . . ?
C1 N3 C5 122.8(4) . . ?
N3 C1 C2 119.8(6) . . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C4 120.3(5) . . ?
C3 C4 C5 119.0(5) . . ?
C9 C4 C3 121.2(5) . . ?
C9 C4 C5 119.8(5) . . ?
N3 C5 C4 117.9(5) . . ?
N3 C5 C6 122.0(4) . . ?
C4 C5 C6 120.0(5) . . ?
O3 C6 C5 123.1(5) . . ?
O3 C6 C7 119.4(5) . . ?
C7 C6 C5 117.4(5) . . ?
C6 C7 C8 122.9(6) . . ?
C9 C8 C7 119.8(6) . . ?
C8 C9 C4 120.1(5) . . ?
N2 C10 C11 126.9(6) . . ?
C12 C11 C10 118.2(6) . . ?
C11 C12 C13 119.2(5) . . ?
C12 C13 C14 123.7(5) . . ?
C12 C13 C21 118.6(5) . . ?
C21 C13 C14 117.7(6) . . ?
C15 C14 C13 122.2(6) . . ?
C14 C15 C16 120.8(6) . . ?
C17 C16 C15 122.4(5) . . ?
C17 C16 C20 117.9(5) . . ?
C20 C16 C15 119.6(6) . . ?
C18 C17 C16 119.4(5) . . ?
C17 C18 C19 118.8(6) . . ?
N1 C19 C18 124.5(5) . . ?
N1 C20 C16 122.1(5) . . ?
N1 C20 C21 118.3(4) . . ?
C16 C20 C21 119.6(5) . . ?
N2 C21 C13 121.6(5) . . ?
N2 C21 C20 118.2(4) . . ?
C13 C21 C20 120.1(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
Dy1 Cl1 2.6631(14) . ?
Dy1 Cl2 2.6574(14) . ?
Dy1 O1 2.425(3) . ?
Dy1 O2 2.223(3) . ?
Dy1 O3 2.164(3) . ?
Dy1 N1 2.556(4) . ?
Dy1 N2 2.563(4) . ?
O2 N3 1.330(5) . ?
O3 C6 1.314(6) . ?
N1 C19 1.314(7) . ?
N1 C20 1.367(6) . ?
N2 C10 1.325(6) . ?
N2 C21 1.368(6) . ?
N3 C1 1.338(6) . ?
N3 C5 1.372(7) . ?
C1 C2 1.398(8) . ?
C2 C3 1.357(8) . ?
C3 C4 1.405(8) . ?
C4 C5 1.418(7) . ?
C4 C9 1.402(8) . ?
C5 C6 1.437(7) . ?
C6 C7 1.375(8) . ?
C7 C8 1.401(8) . ?
C8 C9 1.381(9) . ?
C10 C11 1.360(7) . ?
C11 C12 1.360(8) . ?
C12 C13 1.389(8) . ?
C13 C14 1.445(8) . ?
C13 C21 1.420(7) . ?
C14 C15 1.336(9) . ?
C15 C16 1.433(8) . ?
C16 C17 1.395(8) . ?
C16 C20 1.403(7) . ?
C17 C18 1.360(8) . ?
C18 C19 1.386(7) . ?
C20 C21 1.436(7) . ?
