#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:11:59 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230406 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/74/7057401.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_7057401
loop_
_publ_author_name
'Chu, Xiao-Ya'
'Wang, Wen-Min'
'Nie, Yao-Yao'
'Cui, Jian-Zhong'
'Gao, Hong-Ling'
_publ_section_title
;
 Regulating the luminescent and magnetic properties of rare-earth
 complexes with β-diketonate coligands
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11417
_journal_paper_doi               10.1039/C8NJ01355A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C32 H40 N6 O12 Yb2'
_chemical_formula_sum            'C32 H40 N6 O12 Yb2'
_chemical_formula_weight         1046.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-04-30 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                101.692(2)
_cell_angle_beta                 111.471(2)
_cell_angle_gamma                99.058(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8093(19)
_cell_length_b                   10.5348(19)
_cell_length_c                   11.064(2)
_cell_measurement_reflns_used    3498
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     905.0(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11746
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         3.222
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.5740
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4105
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0149
_refine_ls_R_factor_gt           0.0142
_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)+(0.0195P)²+0.3455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4105
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj01355a2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7057395--7057405.cif.'
_cod_database_code               7057401
_shelx_shelxl_version_number     2017/1
_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_max   0.574
_shelx_estimated_absorpt_t_min   0.423
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6 of O6
 At 1.5 times of:
  All C(H,H,H) groups, H3 of O3
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C13(H13)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
3.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Yb1 Yb 0.99442(2) 0.11517(2) 0.15580(2) 0.01282(3) Uani 1 1 d .
O1 O 0.90364(19) 0.27656(15) 0.23956(16) 0.0192(3) Uani 1 1 d .
O2 O 0.85337(17) -0.07221(14) -0.03062(14) 0.0140(3) Uani 1 1 d .
O3 O 0.8000(2) -0.44069(16) -0.22972(18) 0.0266(4) Uani 1 1 d .
H3 H 0.869849 -0.437494 -0.264941 0.040 Uiso 1 1 calc GR
O4 O 1.1762(2) 0.19021(16) 0.38155(15) 0.0212(3) Uani 1 1 d .
O5 O 1.0701(2) -0.06698(16) 0.22293(15) 0.0205(3) Uani 1 1 d .
O6 O 0.8348(2) 0.18379(16) -0.03519(16) 0.0220(3) Uani 1 1 d D
H6 H 0.861(4) 0.153(3) -0.099(2) 0.026 Uiso 1 1 d DR
N1 N 0.7267(2) 0.00050(17) 0.13789(17) 0.0151(3) Uani 1 1 d .
N2 N 0.6668(2) -0.13709(17) 0.06160(18) 0.0161(3) Uani 1 1 d .
N3 N 0.8118(2) -0.31189(18) -0.15862(18) 0.0177(4) Uani 1 1 d .
C1 C 0.7931(3) 0.2880(2) 0.2924(2) 0.0172(4) Uani 1 1 d .
C2 C 0.8042(3) 0.4150(2) 0.3728(2) 0.0207(4) Uani 1 1 d .
H2 H 0.890191 0.490037 0.386084 0.025 Uiso 1 1 calc R
C3 C 0.6931(3) 0.4325(2) 0.4325(2) 0.0241(5) Uani 1 1 d .
H3A H 0.705656 0.518593 0.487820 0.029 Uiso 1 1 calc R
C4 C 0.5632(3) 0.3260(3) 0.4127(2) 0.0254(5) Uani 1 1 d .
H4 H 0.487202 0.338568 0.454052 0.030 Uiso 1 1 calc R
C5 C 0.5462(3) 0.2013(2) 0.3319(2) 0.0217(4) Uani 1 1 d .
H5 H 0.456029 0.128830 0.316790 0.026 Uiso 1 1 calc R
C6 C 0.6592(3) 0.1786(2) 0.2711(2) 0.0170(4) Uani 1 1 d .
C7 C 0.6264(3) 0.0434(2) 0.1879(2) 0.0173(4) Uani 1 1 d .
H7 H 0.523713 -0.018186 0.168762 0.021 Uiso 1 1 calc R
C8 C 0.7450(3) -0.1615(2) -0.0166(2) 0.0144(4) Uani 1 1 d .
C9 C 0.7159(3) -0.3030(2) -0.0950(2) 0.0159(4) Uani 1 1 d .
C10 C 0.5951(3) -0.4156(2) -0.0907(2) 0.0229(5) Uani 1 1 d .
H10A H 0.584554 -0.498059 -0.156311 0.034 Uiso 1 1 calc GR
H10B H 0.484702 -0.395659 -0.113302 0.034 Uiso 1 1 calc GR
H10C H 0.636441 -0.427322 0.000454 0.034 Uiso 1 1 calc GR
C11 C 1.3116(4) 0.2299(3) 0.6199(3) 0.0403(7) Uani 1 1 d .
H11A H 1.430483 0.259217 0.636592 0.060 Uiso 1 1 calc GR
H11B H 1.302050 0.182001 0.685083 0.060 Uiso 1 1 calc GR
H11C H 1.265441 0.308237 0.630152 0.060 Uiso 1 1 calc GR
C12 C 1.2139(3) 0.1377(3) 0.4777(2) 0.0248(5) Uani 1 1 d .
C13 C 1.1757(3) -0.0011(3) 0.4606(2) 0.0291(5) Uani 1 1 d .
H13 H 1.196360 -0.031307 0.539093 0.035 Uiso 1 1 calc R
C14 C 1.1100(3) -0.0959(2) 0.3366(2) 0.0231(5) Uani 1 1 d .
C15 C 1.0851(4) -0.2429(3) 0.3284(3) 0.0371(6) Uani 1 1 d .
H15A H 0.971311 -0.292190 0.261296 0.056 Uiso 1 1 calc GR
H15B H 1.099182 -0.254846 0.417165 0.056 Uiso 1 1 calc GR
H15C H 1.168539 -0.277288 0.301533 0.056 Uiso 1 1 calc GR
C16 C 0.7815(4) 0.3037(3) -0.0445(3) 0.0310(6) Uani 1 1 d .
H16A H 0.738415 0.329422 0.024488 0.047 Uiso 1 1 calc GR
H16B H 0.692195 0.288500 -0.134563 0.047 Uiso 1 1 calc GR
H16C H 0.877384 0.375554 -0.029647 0.047 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'
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'
Yb Yb -0.3850 5.5486 '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
O1 Yb1 Yb1 148.80(4) . 2_755
O1 Yb1 O2 140.67(5) . 2_755
O1 Yb1 O2 130.69(5) . .
O1 Yb1 O4 75.78(6) . .
O1 Yb1 O5 133.34(6) . .
O1 Yb1 O6 75.37(6) . .
O1 Yb1 N1 77.05(6) . .
O1 Yb1 N3 78.96(6) . 2_755
O1 Yb1 C8 119.83(6) . .
O2 Yb1 Yb1 33.95(4) 2_755 2_755
O2 Yb1 Yb1 33.31(3) . 2_755
O2 Yb1 O2 67.26(6) 2_755 .
O2 Yb1 O4 108.71(6) 2_755 .
O2 Yb1 O5 82.47(5) 2_755 .
O2 Yb1 O6 81.65(5) 2_755 .
O2 Yb1 O6 70.92(5) . .
O2 Yb1 N1 132.75(5) 2_755 .
O2 Yb1 N1 65.56(5) . .
O2 Yb1 N3 123.62(5) . 2_755
O2 Yb1 N3 64.37(5) 2_755 2_755
O2 Yb1 C8 22.51(5) . .
O2 Yb1 C8 87.55(5) 2_755 .
O4 Yb1 Yb1 133.34(4) . 2_755
O4 Yb1 O2 144.90(5) . .
O4 Yb1 O6 144.18(6) . .
O4 Yb1 N1 108.11(6) . .
O4 Yb1 N3 78.97(6) . 2_755
O4 Yb1 C8 130.84(5) . .
O5 Yb1 Yb1 75.00(4) . 2_755
O5 Yb1 O2 72.64(5) . .
O5 Yb1 O4 72.27(6) . .
O5 Yb1 O6 143.49(6) . .
O5 Yb1 N1 81.57(6) . .
O5 Yb1 N3 125.59(6) . 2_755
O5 Yb1 C8 64.15(6) . .
O6 Yb1 Yb1 73.48(4) . 2_755
O6 Yb1 N3 75.06(6) . 2_755
O6 Yb1 C8 82.51(6) . .
N1 Yb1 Yb1 98.84(4) . 2_755
N1 Yb1 O6 85.50(6) . .
N1 Yb1 N3 152.24(6) . 2_755
N1 Yb1 C8 45.63(6) . .
N3 Yb1 Yb1 94.46(4) 2_755 2_755
N3 Yb1 C8 145.98(6) 2_755 .
C8 Yb1 Yb1 54.21(4) . 2_755
C1 O1 Yb1 136.68(14) . .
Yb1 O2 Yb1 112.74(6) 2_755 .
C8 O2 Yb1 114.57(12) . .
C8 O2 Yb1 125.89(12) . 2_755
N3 O3 H3 109.5 . .
C12 O4 Yb1 134.51(15) . .
C14 O5 Yb1 132.97(15) . .
Yb1 O6 H6 107(2) . .
C16 O6 Yb1 131.57(14) . .
C16 O6 H6 113(2) . .
N2 N1 Yb1 115.95(12) . .
C7 N1 Yb1 130.16(14) . .
C7 N1 N2 113.89(17) . .
C8 N2 N1 109.67(16) . .
O3 N3 Yb1 121.49(13) . 2_755
C9 N3 Yb1 122.64(14) . 2_755
C9 N3 O3 115.87(18) . .
O1 C1 C2 119.1(2) . .
O1 C1 C6 123.21(19) . .
C2 C1 C6 117.67(19) . .
C1 C2 H2 119.2 . .
C3 C2 C1 121.6(2) . .
C3 C2 H2 119.2 . .
C2 C3 H3A 119.6 . .
C2 C3 C4 120.9(2) . .
C4 C3 H3A 119.6 . .
C3 C4 H4 120.5 . .
C5 C4 C3 119.0(2) . .
C5 C4 H4 120.5 . .
C4 C5 H5 119.0 . .
C4 C5 C6 121.9(2) . .
C6 C5 H5 119.0 . .
C1 C6 C7 124.74(18) . .
C5 C6 C1 118.9(2) . .
C5 C6 C7 116.3(2) . .
N1 C7 C6 124.74(19) . .
N1 C7 H7 117.6 . .
C6 C7 H7 117.6 . .
O2 C8 Yb1 42.92(9) . .
O2 C8 C9 115.62(17) . .
N2 C8 Yb1 85.90(12) . .
N2 C8 O2 125.44(19) . .
N2 C8 C9 118.91(18) . .
C9 C8 Yb1 148.78(14) . .
N3 C9 C8 111.40(18) . .
N3 C9 C10 126.6(2) . .
C10 C9 C8 121.98(18) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
O4 C12 C11 117.8(2) . .
O4 C12 C13 124.1(2) . .
C13 C12 C11 118.1(2) . .
C12 C13 H13 118.1 . .
C14 C13 C12 123.7(2) . .
C14 C13 H13 118.1 . .
O5 C14 C13 123.7(2) . .
O5 C14 C15 116.1(2) . .
C13 C14 C15 120.1(2) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O6 C16 H16A 109.5 . .
O6 C16 H16B 109.5 . .
O6 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 Yb1 3.8362(6) 2_755
Yb1 O1 2.1728(15) .
Yb1 O2 2.2842(14) 2_755
Yb1 O2 2.3230(14) .
Yb1 O4 2.3023(16) .
Yb1 O5 2.3013(16) .
Yb1 O6 2.3937(16) .
Yb1 N1 2.3928(18) .
Yb1 N3 2.4557(18) 2_755
Yb1 C8 3.102(2) .
O1 C1 1.315(2) .
O2 C8 1.306(2) .
O3 H3 0.8400 .
O3 N3 1.391(2) .
O4 C12 1.259(3) .
O5 C14 1.290(3) .
O6 H6 0.840(10) .
O6 C16 1.424(3) .
N1 N2 1.425(2) .
N1 C7 1.294(3) .
N2 C8 1.300(3) .
N3 C9 1.286(3) .
C1 C2 1.415(3) .
C1 C6 1.426(3) .
C2 H2 0.9500 .
C2 C3 1.382(3) .
C3 H3A 0.9500 .
C3 C4 1.389(4) .
C4 H4 0.9500 .
C4 C5 1.382(3) .
C5 H5 0.9500 .
C5 C6 1.415(3) .
C6 C7 1.450(3) .
C7 H7 0.9500 .
C8 C9 1.494(3) .
C9 C10 1.484(3) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C11 C12 1.511(3) .
C12 C13 1.405(4) .
C13 H13 0.9500 .
C13 C14 1.377(3) .
C14 C15 1.510(3) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
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
O3 H3 O1 0.84 2.29 2.946(2) 134.6 2_755 yes
O6 H6 O5 0.840(10) 1.831(11) 2.664(2) 171(3) 2_755 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Yb1 O1 C1 C2 161.09(16) .
Yb1 O1 C1 C6 -20.0(3) .
Yb1 O2 C8 Yb1 148.81(18) 2_755
Yb1 O2 C8 N2 26.6(3) .
Yb1 O2 C8 N2 175.39(15) 2_755
Yb1 O2 C8 C9 -2.5(2) 2_755
Yb1 O2 C8 C9 -151.29(14) .
Yb1 O4 C12 C11 -166.32(19) .
Yb1 O4 C12 C13 15.8(4) .
Yb1 O5 C14 C13 -25.0(4) .
Yb1 O5 C14 C15 156.48(18) .
Yb1 N1 N2 C8 -19.5(2) .
Yb1 N1 C7 C6 -0.4(3) .
Yb1 N3 C9 C8 -2.7(2) 2_755
Yb1 N3 C9 C10 179.98(17) 2_755
Yb1 C8 C9 N3 -35.9(3) .
Yb1 C8 C9 C10 141.5(2) .
O1 C1 C2 C3 -179.0(2) .
O1 C1 C6 C5 -179.7(2) .
O1 C1 C6 C7 -1.1(3) .
O2 C8 C9 N3 3.2(3) .
O2 C8 C9 C10 -179.36(19) .
O3 N3 C9 C8 177.09(17) .
O3 N3 C9 C10 -0.2(3) .
O4 C12 C13 C14 7.7(4) .
N1 N2 C8 Yb1 13.39(14) .
N1 N2 C8 O2 -4.4(3) .
N1 N2 C8 C9 173.41(17) .
N2 N1 C7 C6 178.94(19) .
N2 C8 C9 N3 -174.80(19) .
N2 C8 C9 C10 2.6(3) .
C1 C2 C3 C4 -1.6(4) .
C1 C6 C7 N1 10.0(3) .
C2 C1 C6 C5 -0.8(3) .
C2 C1 C6 C7 177.8(2) .
C2 C3 C4 C5 -0.1(4) .
C3 C4 C5 C6 1.3(4) .
C4 C5 C6 C1 -0.9(3) .
C4 C5 C6 C7 -179.6(2) .
C5 C6 C7 N1 -171.4(2) .
C6 C1 C2 C3 2.0(3) .
C7 N1 N2 C8 161.12(18) .
C11 C12 C13 C14 -170.1(3) .
C12 C13 C14 O5 -3.1(4) .
C12 C13 C14 C15 175.4(3) .
