#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:22:24 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232855 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/82/4348268.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_4348268
loop_
_publ_author_name
'Wang, Yan-Ning'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 In situ synthesis and structural characterization of a series of
 acylhydrazidate-extended Ln3+and Zn2+coordination polymers
;
_journal_issue                   9
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              673
_journal_paper_doi               10.1039/C4QI00100A
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C27 H26 Dy N9 O7'
_chemical_formula_weight         751.07
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.851(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.586(3)
_cell_length_b                   9.0348(5)
_cell_length_c                   18.2097(11)
_cell_measurement_temperature    293(2)
_cell_volume                     5810.6(7)
_computing_cell_refinement       'Bruker SMAR'
_computing_data_collection       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15947
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.634
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0535P)²+28.1176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4402
_reflns_number_total             5117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00100a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5810.5(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4348268
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Dy1 Dy 0.414390(7) 1.03731(3) 0.383752(14) 0.01680(11) Uani 1 1 d .
O1 O 0.35147(12) 1.0778(5) 0.3003(2) 0.0284(10) Uani 1 1 d .
O2 O 0.29078(19) 1.3426(13) 0.0057(4) 0.143(5) Uani 1 1 d .
O3 O 0.45315(12) 0.9956(5) 0.5269(2) 0.0267(9) Uani 1 1 d .
O4 O 0.40740(14) 1.0771(6) 0.7596(3) 0.0392(12) Uani 1 1 d .
O5 O 0.41400(13) 1.2721(4) 0.4317(3) 0.0337(10) Uani 1 1 d .
O6 O 0.45719(12) 1.8252(4) 0.4115(3) 0.0284(10) Uani 1 1 d .
OW1 O 0.47495(11) 1.1299(4) 0.4016(2) 0.0260(9) Uani 1 1 d .
N1 N 0.30057(15) 1.1304(7) 0.1804(3) 0.0417(15) Uani 1 1 d .
N2 N 0.28752(18) 1.2036(10) 0.1056(4) 0.076(3) Uani 1 1 d .
H2A H 0.2637 1.1947 0.0738 0.092 Uiso 1 1 calc R
N3 N 0.39880(15) 1.2308(6) 0.2587(3) 0.0332(13) Uani 1 1 d .
N4 N 0.46727(15) 1.0169(7) 0.6612(3) 0.0331(13) Uani 1 1 d .
N5 N 0.45297(16) 1.0377(7) 0.7176(3) 0.0360(14) Uani 1 1 d .
H5A H 0.4693 1.0333 0.7686 0.043 Uiso 1 1 calc R
N6 N 0.37885(14) 1.0447(6) 0.4764(3) 0.0253(11) Uani 1 1 d .
N7 N 0.45850(16) 1.4315(5) 0.4361(4) 0.0345(13) Uani 1 1 d .
N8 N 0.46689(16) 1.5780(5) 0.4261(4) 0.0333(13) Uani 1 1 d .
H8A H 0.4893 1.5934 0.4310 0.040 Uiso 1 1 calc R
N9 N 0.38191(14) 1.7806(5) 0.3706(3) 0.0229(11) Uani 1 1 d .
C1 C 0.4213(2) 1.3053(10) 0.2361(4) 0.056(2) Uani 1 1 d .
H1B H 0.4470 1.3056 0.2724 0.067 Uiso 1 1 calc R
C2 C 0.4098(3) 1.3839(15) 0.1623(6) 0.099(5) Uani 1 1 d D
C3 C 0.3709(3) 1.3736(15) 0.1072(6) 0.098(5) Uani 1 1 d .
H3A H 0.3616 1.4167 0.0553 0.118 Uiso 1 1 calc R
C4 C 0.3468(2) 1.2997(11) 0.1301(5) 0.060(3) Uani 1 1 d .
C5 C 0.36159(18) 1.2294(8) 0.2060(4) 0.0335(15) Uani 1 1 d .
C6 C 0.33664(17) 1.1426(7) 0.2296(4) 0.0286(14) Uani 1 1 d .
C7 C 0.3063(2) 1.2853(14) 0.0754(5) 0.084(4) Uani 1 1 d .
C8 C 0.4318(5) 1.5117(16) 0.1528(13) 0.231(15) Uani 1 1 d D
H8B H 0.4470 1.5639 0.2037 0.277 Uiso 1 1 calc R
H8C H 0.4166 1.5800 0.1092 0.277 Uiso 1 1 calc R
C9 C 0.4537(5) 1.4012(17) 0.1285(8) 0.158(9) Uani 1 1 d D
H9B H 0.4722 1.4524 0.1176 0.237 Uiso 1 1 calc R
H9C H 0.4366 1.3490 0.0800 0.237 Uiso 1 1 calc R
H9D H 0.4662 1.3320 0.1726 0.237 Uiso 1 1 calc R
C10 C 0.34284(18) 1.0723(8) 0.4538(4) 0.0344(16) Uani 1 1 d .
H10A H 0.3266 1.0739 0.3977 0.041 Uiso 1 1 calc R
C11 C 0.32694(15) 1.0997(10) 0.5081(4) 0.0431(18) Uani 1 1 d D
C12 C 0.35178(19) 1.0985(9) 0.5913(4) 0.0389(17) Uani 1 1 d .
H12A H 0.3430 1.1164 0.6300 0.047 Uiso 1 1 calc R
C13 C 0.38978(18) 1.0705(7) 0.6164(4) 0.0272(14) Uani 1 1 d .
C14 C 0.40288(17) 1.0456(7) 0.5580(3) 0.0240(13) Uani 1 1 d .
C15 C 0.44250(17) 1.0185(7) 0.5827(3) 0.0242(13) Uani 1 1 d .
C16 C 0.41714(19) 1.0638(7) 0.7031(4) 0.0296(15) Uani 1 1 d .
C17 C 0.28502(17) 1.1201(15) 0.4760(5) 0.084(4) Uani 1 1 d D
H17A H 0.2794 1.1339 0.5222 0.101 Uiso 1 1 calc R
H17B H 0.2723 1.0306 0.4475 0.101 Uiso 1 1 calc R
C18 C 0.2692(5) 1.2501(19) 0.4180(12) 0.202(10) Uani 1 1 d D
H18A H 0.2425 1.2570 0.3999 0.303 Uiso 1 1 calc R
H18B H 0.2740 1.2361 0.3712 0.303 Uiso 1 1 calc R
H18C H 0.2813 1.3396 0.4460 0.303 Uiso 1 1 calc R
C19 C 0.34560(18) 1.7511(7) 0.3492(4) 0.0304(14) Uani 1 1 d .
H19A H 0.3287 1.8300 0.3335 0.037 Uiso 1 1 calc R
C20 C 0.33124(14) 1.6092(8) 0.3488(4) 0.0345(15) Uani 1 1 d D
C21 C 0.35640(19) 1.4942(7) 0.3719(4) 0.0323(15) Uani 1 1 d .
H21A H 0.3481 1.3984 0.3731 0.039 Uiso 1 1 calc R
C22 C 0.39466(18) 1.5200(6) 0.3939(4) 0.0244(13) Uani 1 1 d .
C23 C 0.40549(17) 1.6655(6) 0.3905(3) 0.0232(13) Uani 1 1 d .
C24 C 0.44477(17) 1.6977(6) 0.4100(3) 0.0228(12) Uani 1 1 d .
C25 C 0.42356(18) 1.4036(7) 0.4216(4) 0.0302(14) Uani 1 1 d .
C26 C 0.28962(15) 1.5897(8) 0.3214(5) 0.050(2) Uani 1 1 d D
H26A H 0.2771 1.6835 0.3000 0.060 Uiso 1 1 calc R
H26B H 0.2859 1.5656 0.3692 0.060 Uiso 1 1 calc R
C27 C 0.2704(4) 1.4719(16) 0.2567(10) 0.153(8) Uani 1 1 d D
H27A H 0.2441 1.4672 0.2434 0.229 Uiso 1 1 calc R
H27B H 0.2821 1.3777 0.2775 0.229 Uiso 1 1 calc R
H27C H 0.2730 1.4960 0.2081 0.229 Uiso 1 1 calc R
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'
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
O1 Dy1 O5 84.99(16) . .
O1 Dy1 O3 136.25(14) . .
O5 Dy1 O3 80.89(15) . .
O1 Dy1 O4 79.29(16) . 6_575
O5 Dy1 O4 137.96(17) . 6_575
O3 Dy1 O4 135.23(16) . 6_575
O1 Dy1 OW1 138.62(14) . .
O5 Dy1 OW1 78.80(15) . .
O3 Dy1 OW1 78.34(14) . .
O4 Dy1 OW1 87.77(15) 6_575 .
O1 Dy1 O6 134.84(15) . 1_545
O5 Dy1 O6 139.95(15) . 1_545
O3 Dy1 O6 66.92(14) . 1_545
O4 Dy1 O6 68.31(16) 6_575 1_545
OW1 Dy1 O6 72.07(14) . 1_545
O1 Dy1 N9 74.78(15) . 1_545
O5 Dy1 N9 140.20(16) . 1_545
O3 Dy1 N9 90.42(15) . 1_545
O4 Dy1 N9 71.71(16) 6_575 1_545
OW1 Dy1 N9 137.47(14) . 1_545
O6 Dy1 N9 65.83(14) 1_545 1_545
O1 Dy1 N6 71.68(15) . .
O5 Dy1 N6 68.70(16) . .
O3 Dy1 N6 64.60(15) . .
O4 Dy1 N6 138.51(16) 6_575 .
OW1 Dy1 N6 133.40(14) . .
O6 Dy1 N6 113.95(15) 1_545 .
N9 Dy1 N6 72.48(15) 1_545 .
O1 Dy1 N3 64.68(15) . .
O5 Dy1 N3 71.69(16) . .
O3 Dy1 N3 144.13(16) . .
O4 Dy1 N3 66.33(17) 6_575 .
OW1 Dy1 N3 74.09(14) . .
O6 Dy1 N3 123.38(16) 1_545 .
N9 Dy1 N3 125.44(15) 1_545 .
N6 Dy1 N3 122.36(16) . .
C6 O1 Dy1 127.2(4) . .
C15 O3 Dy1 124.2(4) . .
C16 O4 Dy1 141.9(4) . 6_576
C25 O5 Dy1 138.3(4) . .
C24 O6 Dy1 119.2(4) . 1_565
C6 N1 N2 116.2(6) . .
C7 N2 N1 129.9(6) . .
C1 N3 C5 117.2(5) . .
C1 N3 Dy1 131.3(5) . .
C5 N3 Dy1 110.6(4) . .
C15 N4 N5 116.6(5) . .
C16 N5 N4 128.7(5) . .
C10 N6 C14 117.7(5) . .
C10 N6 Dy1 128.3(4) . .
C14 N6 Dy1 112.9(4) . .
C25 N7 N8 116.6(5) . .
C24 N8 N7 128.6(6) . .
C23 N9 C19 116.9(5) . .
C23 N9 Dy1 114.4(4) . 1_565
C19 N9 Dy1 128.7(4) . 1_565
N3 C1 C2 125.8(7) . .
C1 C2 C3 115.2(7) . .
C1 C2 C8 123.1(12) . .
C3 C2 C8 118.1(11) . .
C4 C3 C2 120.0(7) . .
C3 C4 C5 119.1(7) . .
C3 C4 C7 122.3(7) . .
C5 C4 C7 118.5(7) . .
N3 C5 C4 122.6(6) . .
N3 C5 C6 117.4(5) . .
C4 C5 C6 119.9(6) . .
O1 C6 N1 120.8(6) . .
O1 C6 C5 118.1(5) . .
N1 C6 C5 121.1(5) . .
O2 C7 N2 122.8(8) . .
O2 C7 C4 122.7(8) . .
N2 C7 C4 114.5(6) . .
C2 C8 C9 87.9(12) . .
N6 C10 C11 125.2(6) . .
C12 C11 C10 116.3(5) . .
C12 C11 C17 122.8(6) . .
C10 C11 C17 120.9(6) . .
C13 C12 C11 119.5(6) . .
C12 C13 C14 120.0(6) . .
C12 C13 C16 122.1(6) . .
C14 C13 C16 117.9(6) . .
N6 C14 C13 121.2(6) . .
N6 C14 C15 117.7(5) . .
C13 C14 C15 121.1(5) . .
O3 C15 N4 120.5(6) . .
O3 C15 C14 118.8(5) . .
N4 C15 C14 120.7(5) . .
O4 C16 N5 122.9(6) . .
O4 C16 C13 122.0(6) . .
N5 C16 C13 115.0(5) . .
C11 C17 C18 113.7(10) . .
N9 C19 C20 124.4(5) . .
C21 C20 C19 117.1(5) . .
C21 C20 C26 123.4(6) . .
C19 C20 C26 119.4(6) . .
C20 C21 C22 120.3(6) . .
C23 C22 C21 117.3(6) . .
C23 C22 C25 119.0(6) . .
C21 C22 C25 123.7(6) . .
N9 C23 C22 123.8(6) . .
N9 C23 C24 116.7(5) . .
C22 C23 C24 119.5(5) . .
O6 C24 N8 121.9(6) . .
O6 C24 C23 123.7(5) . .
N8 C24 C23 114.4(5) . .
O5 C25 N7 120.1(6) . .
O5 C25 C22 118.5(6) . .
N7 C25 C22 121.4(6) . .
C20 C26 C27 115.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.286(4) .
Dy1 O5 2.297(4) .
Dy1 O3 2.383(4) .
Dy1 O4 2.386(4) 6_575
Dy1 OW1 2.418(4) .
Dy1 O6 2.455(4) 1_545
Dy1 N9 2.610(5) 1_545
Dy1 N6 2.640(5) .
Dy1 N3 2.712(5) .
O1 C6 1.289(7) .
O2 C7 1.246(9) .
O3 C15 1.280(7) .
O4 C16 1.257(7) .
O4 Dy1 2.386(4) 6_576
O5 C25 1.285(8) .
O6 C24 1.248(7) .
O6 Dy1 2.455(4) 1_565
N1 C6 1.303(8) .
N1 N2 1.388(8) .
N2 C7 1.328(11) .
N3 C1 1.321(9) .
N3 C5 1.347(8) .
N4 C15 1.319(8) .
N4 N5 1.391(7) .
N5 C16 1.341(9) .
N6 C10 1.317(8) .
N6 C14 1.356(7) .
N7 C25 1.310(9) .
N7 N8 1.396(7) .
N8 C24 1.338(8) .
N9 C23 1.333(7) .
N9 C19 1.336(8) .
N9 Dy1 2.610(5) 1_565
C1 C2 1.402(11) .
C2 C3 1.411(12) .
C2 C8 1.5015(11) .
C3 C4 1.376(11) .
C4 C5 1.388(9) .
C4 C7 1.463(10) .
C5 C6 1.469(9) .
C8 C9 1.5135(10) .
C10 C11 1.412(9) .
C11 C12 1.384(9) .
C11 C17 1.5012(10) .
C12 C13 1.383(9) .
C13 C14 1.395(8) .
C13 C16 1.457(9) .
C14 C15 1.444(9) .
C17 C18 1.5136(10) .
C19 C20 1.401(9) .
C20 C21 1.367(9) .
C20 C26 1.5009(10) .
C21 C22 1.400(9) .
C22 C23 1.393(8) .
C22 C25 1.465(9) .
C23 C24 1.460(8) .
C26 C27 1.5138(10) .
