#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:28:26 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229102 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/06/7230603.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_7230603
loop_
_publ_author_name
'Yu, Qi'
'Dong, Hong'
'Zhang, Xin'
'Zhu, Ya-Xin'
'Wang, Jian-Hui'
'Zhang, Feng-Ming'
'Sun, Xiao-Jun'
_publ_section_title
;
 Novel stable metal--organic framework photocatalyst for light-driven
 hydrogen production
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3228
_journal_paper_doi               10.1039/C8CE00386F
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C8 H6 Dy N O6, H2 O'
_chemical_formula_sum            'C8 H8 Dy N O7'
_chemical_formula_weight         392.65
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-17 deposited with the CCDC.
2018-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.241(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.55760(10)
_cell_length_b                   16.2048(4)
_cell_length_c                   14.0456(3)
_cell_measurement_reflns_used    2379
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9595
_cell_measurement_theta_min      2.8995
_cell_volume                     1033.00(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4200
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    7.258
_exptl_absorpt_correction_T_max  0.4090
_exptl_absorpt_correction_T_min  0.3717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1822
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0174P)²+1.1671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0467
_reflns_number_gt                1563
_reflns_number_total             1822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00386f2.cif
_cod_data_source_block           fm2
_cod_depositor_comments          'Adding full bibliography for 7230603.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7230603
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.0659(9) 0.6644(2) 0.5969(3) 0.0128(9) Uani 1 1 d .
C2 C 0.2162(9) 0.6351(2) 0.6801(3) 0.0132(9) Uani 1 1 d .
H2 H 0.3651 0.6667 0.7118 0.016 Uiso 1 1 calc R
C3 C 0.1453(9) 0.5585(2) 0.7166(3) 0.0136(9) Uani 1 1 d .
C4 C -0.0705(9) 0.5106(3) 0.6665(3) 0.0159(9) Uani 1 1 d .
H4 H -0.1170 0.4589 0.6896 0.019 Uiso 1 1 calc R
C5 C -0.2157(8) 0.5396(2) 0.5824(3) 0.0145(9) Uani 1 1 d .
C6 C -0.1492(9) 0.6167(3) 0.5476(3) 0.0151(9) Uani 1 1 d .
H6 H -0.2489 0.6364 0.4914 0.018 Uiso 1 1 calc R
C7 C 0.1300(9) 0.7485(2) 0.5612(3) 0.0151(9) Uani 1 1 d .
C8 C 0.2957(9) 0.5302(2) 0.8098(3) 0.0134(9) Uani 1 1 d .
N1 N -0.4367(8) 0.4859(2) 0.5374(2) 0.0179(8) Uani 1 1 d .
O1 O 0.3246(7) 0.79319(17) 0.6055(2) 0.0269(8) Uani 1 1 d .
O2 O -0.0126(6) 0.77596(17) 0.4869(2) 0.0216(7) Uani 1 1 d .
O3 O 0.5095(6) 0.57272(16) 0.8458(2) 0.0158(7) Uani 1 1 d .
O4 O 0.1976(6) 0.46684(17) 0.8482(2) 0.0185(7) Uani 1 1 d .
O5 O 0.4836(6) 0.82356(18) 0.3938(2) 0.0205(7) Uani 1 1 d D
H51 H 0.652(5) 0.805(2) 0.412(3) 0.031 Uiso 1 1 d D
H52 H 0.393(7) 0.790(2) 0.355(3) 0.031 Uiso 1 1 d D
O6 O 0.2505(6) 1.05504(18) 0.47008(19) 0.0112(6) Uani 1 1 d D
H61 H 0.235(9) 1.056(3) 0.4097(8) 0.017 Uiso 1 1 d D
O7 O 0.2359(16) 0.7021(3) 0.2714(4) 0.120(3) Uani 1 1 d D
H71 H 0.400(11) 0.679(6) 0.266(7) 0.180 Uiso 1 1 d D
H72 H 0.129(17) 0.700(6) 0.219(4) 0.180 Uiso 1 1 d D
Dy1 Dy 0.24138(4) 0.908755(11) 0.496847(13) 0.00947(8) 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'
O O 0.0106 0.0060 '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'
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
C6 C1 C2 120.3(4) . .
C6 C1 C7 119.6(4) . .
C2 C1 C7 120.0(4) . .
C1 C2 C3 120.2(4) . .
C1 C2 H2 119.9 . .
C3 C2 H2 119.9 . .
C2 C3 C4 119.2(4) . .
C2 C3 C8 119.5(4) . .
C4 C3 C8 121.3(4) . .
C5 C4 C3 120.2(4) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.3(4) . .
C4 C5 N1 115.7(4) . .
C6 C5 N1 124.0(4) . .
C1 C6 C5 119.7(4) . .
C1 C6 H6 120.2 . .
C5 C6 H6 120.2 . .
O2 C7 O1 119.4(4) . .
O2 C7 C1 120.0(4) . .
O1 C7 C1 120.6(4) . .
O2 C7 Dy1 60.1(2) . .
O1 C7 Dy1 59.3(2) . .
C1 C7 Dy1 178.7(3) . .
O4 C8 O3 124.4(4) . .
O4 C8 C3 118.2(3) . .
O3 C8 C3 117.4(4) . .
N1 N1 C5 113.9(4) 3_466 .
C7 O1 Dy1 94.0(2) . .
C7 O2 Dy1 93.3(2) . .
C8 O3 Dy1 135.5(3) . 4_676
C8 O4 Dy1 134.6(3) . 2_546
Dy1 O5 H51 119(3) . .
Dy1 O5 H52 123(3) . .
H51 O5 H52 110.2(17) . .
Dy1 O6 Dy1 104.01(10) 3_676 .
Dy1 O6 Dy1 143.70(13) 3_676 3_576
Dy1 O6 Dy1 100.42(10) . 3_576
Dy1 O6 H61 100(3) 3_676 .
Dy1 O6 H61 100(3) . .
Dy1 O6 H61 101(3) 3_576 .
H71 O7 H72 110.6(19) . .
O3 Dy1 O5 73.18(10) 4_575 .
O3 Dy1 O4 143.32(9) 4_575 2_556
O5 Dy1 O4 141.20(10) . 2_556
O3 Dy1 O6 120.11(10) 4_575 3_676
O5 Dy1 O6 76.27(10) . 3_676
O4 Dy1 O6 72.14(10) 2_556 3_676
O3 Dy1 O6 74.93(9) 4_575 .
O5 Dy1 O6 117.92(10) . .
O4 Dy1 O6 75.45(9) 2_556 .
O6 Dy1 O6 75.99(10) 3_676 .
O3 Dy1 O6 77.79(10) 4_575 3_576
O5 Dy1 O6 139.65(10) . 3_576
O4 Dy1 O6 76.01(9) 2_556 3_576
O6 Dy1 O6 143.70(13) 3_676 3_576
O6 Dy1 O6 79.58(10) . 3_576
O3 Dy1 O1 135.52(10) 4_575 .
O5 Dy1 O1 83.03(11) . .
O4 Dy1 O1 74.30(10) 2_556 .
O6 Dy1 O1 88.52(10) 3_676 .
O6 Dy1 O1 149.02(9) . .
O6 Dy1 O1 99.32(11) 3_576 .
O3 Dy1 O2 83.51(10) 4_575 .
O5 Dy1 O2 72.16(11) . .
O4 Dy1 O2 114.76(10) 2_556 .
O6 Dy1 O2 132.27(10) 3_676 .
O6 Dy1 O2 151.19(9) . .
O6 Dy1 O2 77.31(10) 3_576 .
O1 Dy1 O2 53.21(9) . .
O3 Dy1 C7 109.62(11) 4_575 .
O5 Dy1 C7 76.35(12) . .
O4 Dy1 C7 94.66(11) 2_556 .
O6 Dy1 C7 111.35(11) 3_676 .
O6 Dy1 C7 165.60(11) . .
O6 Dy1 C7 87.95(11) 3_576 .
O1 Dy1 C7 26.65(10) . .
O2 Dy1 C7 26.56(10) . .
O3 Dy1 Dy1 72.13(7) 4_575 3_576
O5 Dy1 Dy1 143.19(8) . 3_576
O4 Dy1 Dy1 71.29(7) 2_556 3_576
O6 Dy1 Dy1 111.55(7) 3_676 3_576
O6 Dy1 Dy1 39.81(6) . 3_576
O6 Dy1 Dy1 39.77(7) 3_576 3_576
O1 Dy1 Dy1 131.53(8) . 3_576
O2 Dy1 Dy1 115.27(7) . 3_576
C7 Dy1 Dy1 127.35(9) . 3_576
O3 Dy1 Dy1 98.77(7) 4_575 3_676
O5 Dy1 Dy1 98.47(7) . 3_676
O4 Dy1 Dy1 69.27(7) 2_556 3_676
O6 Dy1 Dy1 38.07(7) 3_676 3_676
O6 Dy1 Dy1 37.92(6) . 3_676
O6 Dy1 Dy1 113.30(7) 3_576 3_676
O1 Dy1 Dy1 121.91(7) . 3_676
O2 Dy1 Dy1 169.38(7) . 3_676
C7 Dy1 Dy1 147.80(8) . 3_676
Dy1 Dy1 Dy1 75.191(7) 3_576 3_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.383(5) .
C1 C2 1.384(6) .
C1 C7 1.490(5) .
C2 C3 1.392(6) .
C2 H2 0.9300 .
C3 C4 1.393(6) .
C3 C8 1.493(5) .
C4 C5 1.382(6) .
C4 H4 0.9300 .
C5 C6 1.385(6) .
C5 N1 1.434(5) .
C6 H6 0.9300 .
C7 O2 1.259(5) .
C7 O1 1.264(5) .
C7 Dy1 2.812(4) .
C8 O4 1.261(5) .
C8 O3 1.261(5) .
N1 N1 1.237(6) 3_466
O1 Dy1 2.424(3) .
O2 Dy1 2.442(3) .
O3 Dy1 2.301(3) 4_676
O4 Dy1 2.364(3) 2_546
O5 Dy1 2.348(3) .
O5 H51 0.844(10) .
O5 H52 0.849(10) .
O6 Dy1 2.393(3) 3_676
O6 Dy1 2.401(3) .
O6 Dy1 2.403(3) 3_576
O6 H61 0.845(10) .
O7 H71 0.847(11) .
O7 H72 0.847(10) .
Dy1 O3 2.301(3) 4_575
Dy1 O4 2.364(3) 2_556
Dy1 O6 2.393(3) 3_676
Dy1 O6 2.403(3) 3_576
Dy1 Dy1 3.6918(3) 3_576
Dy1 Dy1 3.7778(3) 3_676
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
O5 H51 O2 0.844(10) 1.833(15) 2.651(4) 163(4) 1_655
O5 H52 O7 0.849(10) 1.942(13) 2.784(6) 171(4) .
O6 H61 O4 0.845(10) 2.38(4) 2.801(4) 112(3) 4_675
O7 H72 O1 0.847(10) 2.016(18) 2.855(6) 170(9) 4_575
