#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:09:43 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185171 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/40/7224079.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_7224079
loop_
_publ_author_name
'Zhang, Han'
'Yan, Zhi-Hao'
'Luo, Yun'
'Zheng, Xiu-Ying'
'Kong, Xiang-Jian'
'Long, La-Sheng'
'Zheng, Lan-Sun'
_publ_section_title
;
 Anion-controlled assembly of a series of heterometallic 3d--4f compounds
 with 0D cluster, 1D chain, 2D network and 3D frameworks
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4142
_journal_paper_doi               10.1039/C5CE02503F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C14 H30 Dy N2 Ni O14, Cl, 2(H2 O)'
_chemical_formula_sum            'C14 H34 Cl Dy N2 Ni O16'
_chemical_formula_weight         743.09
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                100.694(5)
_cell_angle_beta                 103.838(4)
_cell_angle_gamma                105.732(5)
_cell_formula_units_Z            2
_cell_length_a                   7.558(2)
_cell_length_b                   11.269(3)
_cell_length_c                   15.561(4)
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.69
_cell_volume                     1193.4(5)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5977
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_T_max  0.6853
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0221P)²+3.9207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                3968
_reflns_number_total             4085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02503f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7224073--7224079.cif.'
_cod_database_code               7224079
_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 O(H,H) groups
2.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B)
2.b Rotating group:
 O10(H10A,H10B), O14(H14A,H14B), O12(H12A,H12B), O11(H11A,H11B), O13(H13A,
 H13B), O9(H9A,H9B)
2.c Ternary CH refined with riding coordinates:
 C5(H5), C10(H10)
2.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C11(H11C,H11D), C6(H6A,H6B), C2(H2A,H2B), C13(H13C,H13D), C9(H9C,
 H9D), C7(H7A,H7B), C8(H8A,H8B)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Dy1 Dy 0.58493(3) 0.750846(17) 0.331017(13) 0.01371(8) Uani 1 1 d .
Ni1 Ni 1.08403(7) 1.23840(5) 0.30663(4) 0.01240(12) Uani 1 1 d .
Cl1 Cl 0.93550(16) 0.66118(11) 0.11959(8) 0.0257(2) Uani 1 1 d .
O10 O 0.3426(4) 0.8262(3) 0.2581(2) 0.0180(6) Uani 1 1 d .
H10A H 0.2431 0.7614 0.2193 0.027 Uiso 1 1 d R
H10B H 0.3885 0.8792 0.2272 0.027 Uiso 1 1 d R
O4 O 0.2880(4) 0.5996(3) 0.2963(2) 0.0180(6) Uani 1 1 d .
O7 O 0.7230(4) 0.8782(3) 0.2444(2) 0.0185(6) Uani 1 1 d .
O1 O 1.0961(4) 1.3246(3) 0.43822(19) 0.0168(6) Uani 1 1 d .
O3 O 1.2730(4) 1.4019(3) 0.3018(2) 0.0160(6) Uani 1 1 d .
O8 O 0.9025(4) 1.0776(3) 0.3205(2) 0.0166(6) Uani 1 1 d .
O14 O 0.5672(4) 0.6134(3) 0.1964(2) 0.0200(7) Uani 1 1 d .
H14A H 0.6453 0.6536 0.1688 0.030 Uiso 1 1 d R
H14B H 0.4477 0.5844 0.1584 0.030 Uiso 1 1 d R
O5 O 1.2800(4) 1.1441(3) 0.3008(2) 0.0198(7) Uani 1 1 d .
O12 O 0.6413(4) 0.5835(3) 0.3942(2) 0.0237(7) Uani 1 1 d .
H12A H 0.5303 0.5231 0.3858 0.036 Uiso 1 1 d R
H12B H 0.7023 0.6137 0.4541 0.036 Uiso 1 1 d R
O15 O 1.2502(5) 0.9746(3) 0.4001(2) 0.0273(8) Uani 1 1 d G
H15A H 1.3155 0.9291 0.3800 0.041 Uiso 1 1 d G
H15B H 1.2369 1.0279 0.3672 0.041 Uiso 1 1 d G
N1 N 0.8804(5) 1.3270(3) 0.2773(2) 0.0124(7) Uani 1 1 d .
O6 O 1.3832(5) 1.0390(3) 0.1981(2) 0.0235(7) Uani 1 1 d .
O2 O 0.8745(4) 1.3303(3) 0.5083(2) 0.0214(7) Uani 1 1 d .
N2 N 0.9778(5) 1.1412(3) 0.1682(2) 0.0132(7) Uani 1 1 d .
O16 O 1.2042(5) 1.4746(3) 0.0917(2) 0.0269(7) Uani 1 1 d G
H16A H 1.1800 1.4441 0.0330 0.040 Uiso 1 1 d G
H16B H 1.1311 1.5203 0.1011 0.040 Uiso 1 1 d G
O11 O 0.4703(5) 0.7814(3) 0.4640(2) 0.0338(9) Uani 1 1 d .
H11A H 0.5622 0.7900 0.5136 0.051 Uiso 1 1 d R
H11B H 0.3708 0.7148 0.4570 0.051 Uiso 1 1 d R
O13 O 0.9147(5) 0.7825(4) 0.3826(3) 0.0362(9) Uani 1 1 d .
H13A H 0.9389 0.7459 0.4270 0.054 Uiso 1 1 d R
H13B H 0.9790 0.8647 0.4033 0.054 Uiso 1 1 d R
C5 C 0.7522(6) 1.2578(4) 0.1822(3) 0.0123(8) Uani 1 1 d .
H5 H 0.6645 1.1758 0.1858 0.015 Uiso 1 1 calc R
C14 C 0.8246(6) 0.9870(4) 0.2482(3) 0.0141(8) Uani 1 1 d .
C4 C 1.1977(6) 1.4882(4) 0.2957(3) 0.0145(8) Uani 1 1 d .
O9 O 0.7013(5) 0.9669(3) 0.4190(2) 0.0331(9) Uani 1 1 d .
H9A H 0.6050 0.9908 0.4293 0.050 Uiso 1 1 d R
H9B H 0.7580 1.0161 0.3889 0.050 Uiso 1 1 d R
C10 C 0.8776(6) 1.2220(4) 0.1244(3) 0.0125(8) Uani 1 1 d .
H10 H 0.9794 1.3031 0.1290 0.015 Uiso 1 1 calc R
C3 C 0.9884(6) 1.4629(4) 0.2895(3) 0.0142(8) Uani 1 1 d .
H3A H 0.9804 1.5150 0.3462 0.017 Uiso 1 1 calc R
H3B H 0.9258 1.4911 0.2372 0.017 Uiso 1 1 calc R
C12 C 1.2848(6) 1.1025(4) 0.2188(3) 0.0178(9) Uani 1 1 d .
C11 C 1.1519(6) 1.1368(4) 0.1435(3) 0.0172(9) Uani 1 1 d .
H11C H 1.2202 1.2210 0.1365 0.021 Uiso 1 1 calc R
H11D H 1.1156 1.0720 0.0842 0.021 Uiso 1 1 calc R
C6 C 0.6245(6) 1.3269(4) 0.1384(3) 0.0176(9) Uani 1 1 d .
H6A H 0.7058 1.4127 0.1394 0.021 Uiso 1 1 calc R
H6B H 0.5360 1.3386 0.1744 0.021 Uiso 1 1 calc R
C2 C 0.7835(6) 1.3142(4) 0.3486(3) 0.0147(8) Uani 1 1 d .
H2A H 0.6791 1.2304 0.3285 0.018 Uiso 1 1 calc R
H2B H 0.7247 1.3823 0.3574 0.018 Uiso 1 1 calc R
C1 C 0.9282(6) 1.3245(4) 0.4388(3) 0.0163(9) Uani 1 1 d .
C13 C 0.8512(6) 1.0114(4) 0.1592(3) 0.0168(9) Uani 1 1 d .
H13C H 0.9055 0.9485 0.1320 0.020 Uiso 1 1 calc R
H13D H 0.7228 0.9965 0.1159 0.020 Uiso 1 1 calc R
C9 C 0.7663(6) 1.1609(4) 0.0222(3) 0.0175(9) Uani 1 1 d .
H9C H 0.8589 1.1550 -0.0126 0.021 Uiso 1 1 calc R
H9D H 0.6809 1.0731 0.0140 0.021 Uiso 1 1 calc R
C7 C 0.5068(6) 1.2525(4) 0.0396(3) 0.0216(10) Uani 1 1 d .
H7A H 0.4229 1.2986 0.0127 0.026 Uiso 1 1 calc R
H7B H 0.4237 1.1670 0.0380 0.026 Uiso 1 1 calc R
C8 C 0.6453(7) 1.2384(4) -0.0160(3) 0.0202(9) Uani 1 1 d .
H8A H 0.5708 1.1947 -0.0812 0.024 Uiso 1 1 calc R
H8B H 0.7308 1.3240 -0.0128 0.024 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'
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'
Ni Ni 0.3393 1.1124 '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
O10 Dy1 O12 144.13(11) .
O10 Dy1 O11 86.80(12) .
O10 Dy1 O9 79.23(12) .
O4 Dy1 O10 70.21(10) .
O4 Dy1 O7 131.56(10) .
O4 Dy1 O14 77.92(11) .
O4 Dy1 O12 74.18(11) .
O4 Dy1 O11 71.81(11) .
O4 Dy1 O13 142.32(11) .
O4 Dy1 O9 129.55(12) .
O7 Dy1 O10 74.19(11) .
O7 Dy1 O12 136.61(11) .
O7 Dy1 O11 137.54(11) .
O7 Dy1 O9 72.04(11) .
O14 Dy1 O10 94.01(11) .
O14 Dy1 O7 72.89(10) .
O14 Dy1 O12 82.56(11) .
O14 Dy1 O11 147.49(11) .
O14 Dy1 O13 88.56(13) .
O14 Dy1 O9 144.81(11) .
O12 Dy1 O11 78.12(13) .
O13 Dy1 O10 146.58(11) .
O13 Dy1 O7 74.81(11) .
O13 Dy1 O12 69.25(11) .
O13 Dy1 O11 108.30(13) .
O13 Dy1 O9 79.65(14) .
O9 Dy1 O12 122.45(12) .
O9 Dy1 O11 67.23(12) .
O1 Ni1 N2 161.47(13) .
O3 Ni1 O1 90.56(12) .
O3 Ni1 O8 176.28(12) .
O3 Ni1 O5 91.24(12) .
O3 Ni1 N1 85.10(13) .
O3 Ni1 N2 100.05(13) .
O8 Ni1 O1 86.19(12) .
O8 Ni1 O5 88.46(12) .
O8 Ni1 N1 96.11(13) .
O8 Ni1 N2 83.57(12) .
O5 Ni1 O1 114.37(12) .
O5 Ni1 N1 165.29(13) .
O5 Ni1 N2 80.80(13) .
N1 Ni1 O1 79.96(13) .
N1 Ni1 N2 85.81(13) .
C4 O4 Dy1 145.9(3) 1_445
C14 O7 Dy1 143.9(3) .
C1 O1 Ni1 109.0(3) .
C4 O3 Ni1 112.1(3) .
C14 O8 Ni1 114.7(3) .
C12 O5 Ni1 113.6(3) .
C5 N1 Ni1 106.7(2) .
C3 N1 Ni1 106.4(2) .
C3 N1 C5 114.5(3) .
C2 N1 Ni1 103.8(2) .
C2 N1 C5 114.0(3) .
C2 N1 C3 110.5(3) .
C10 N2 Ni1 104.1(2) .
C11 N2 Ni1 103.5(3) .
C11 N2 C10 114.7(3) .
C11 N2 C13 110.9(3) .
C13 N2 Ni1 107.8(2) .
C13 N2 C10 114.7(3) .
N1 C5 C10 108.1(3) .
N1 C5 C6 115.0(3) .
C6 C5 C10 112.7(3) .
O7 C14 O8 124.4(4) .
O7 C14 C13 116.9(4) .
O8 C14 C13 118.7(4) .
O4 C4 O3 124.0(4) 1_665
O4 C4 C3 115.2(4) 1_665
O3 C4 C3 120.7(4) .
N2 C10 C5 107.7(3) .
N2 C10 C9 113.7(3) .
C9 C10 C5 113.6(3) .
N1 C3 C4 113.8(3) .
O5 C12 C11 115.2(4) .
O6 C12 O5 125.3(4) .
O6 C12 C11 119.5(4) .
N2 C11 C12 109.5(3) .
C5 C6 C7 111.4(4) .
N1 C2 C1 110.2(3) .
O1 C1 C2 118.1(4) .
O2 C1 O1 123.8(4) .
O2 C1 C2 118.1(4) .
N2 C13 C14 114.7(3) .
C8 C9 C10 111.6(3) .
C6 C7 C8 108.8(4) .
C9 C8 C7 109.8(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O10 2.360(3) .
Dy1 O4 2.289(3) .
Dy1 O7 2.355(3) .
Dy1 O14 2.314(3) .
Dy1 O12 2.372(3) .
Dy1 O11 2.430(3) .
Dy1 O13 2.332(3) .
Dy1 O9 2.367(3) .
Ni1 O1 2.066(3) .
Ni1 O3 2.028(3) .
Ni1 O8 2.037(3) .
Ni1 O5 2.053(3) .
Ni1 N1 2.060(3) .
Ni1 N2 2.075(4) .
O4 C4 1.253(5) 1_445
O7 C14 1.240(5) .
O1 C1 1.271(5) .
O3 C4 1.260(5) .
O8 C14 1.259(5) .
O5 C12 1.287(5) .
N1 C5 1.487(5) .
N1 C3 1.479(5) .
N1 C2 1.476(5) .
O6 C12 1.219(5) .
O2 C1 1.240(5) .
N2 C10 1.491(5) .
N2 C11 1.466(5) .
N2 C13 1.475(5) .
C5 C10 1.534(5) .
C5 C6 1.514(6) .
C14 C13 1.509(6) .
C4 O4 1.253(5) 1_665
C4 C3 1.505(6) .
C10 C9 1.533(6) .
C12 C11 1.532(6) .
C6 C7 1.523(6) .
C2 C1 1.522(6) .
C9 C8 1.522(6) .
C7 C8 1.530(6) .
