#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:43:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179455 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/52/4335250.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_4335250
loop_
_publ_author_name
'Soichiro Sakamoto'
'Takeshi Fujinami'
'Koshiro Nishi'
'Naohide Matsumoto'
'Naotaka Mochida'
'Takayuki Ishida'
'Yukinari Sunatsuki'
'Nazzareno Re'
_publ_section_title
;
 Carbonato-Bridged NiII2LnIII2 (LnIII= GdIII, TbIII, DyIII) Complexes
 Generated by Atmospheric CO2 Fixation and Their Single-Molecule-Magnet
 Behavior: [(μ4-CO3)2{NiII(3-MeOsaltn)(MeOH or H2O)LnIII(NO3)}2].solvent
 [3-MeOsaltn =N,N'-Bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7218
_journal_page_last               7229
_journal_paper_doi               10.1021/ic4008312
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H27 Dy N4 Ni O12'
_chemical_formula_sum            'C22 H27 Dy N4 Ni O12'
_chemical_formula_weight         760.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.0500(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.3437(8)
_cell_length_b                   12.4100(7)
_cell_length_c                   17.3181(9)
_cell_measurement_reflns_used    14932
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.12
_cell_volume                     2603.7(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24135
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.647
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_description       block
_exptl_crystal_F_000             1508.00
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.252
_refine_diff_density_max         2.250
_refine_diff_density_min         -2.830
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0481P)²+23.4539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                4633
_reflns_number_total             5864
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic4008312_si_003_6.cif
_cod_data_source_block           120914(Ni-Dy)
_cod_database_code               4335250
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+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 0.00687(3) 0.14093(3) 0.05488(2) 0.02698(15) Uani 1.0 4 d .
Ni1 Ni -0.22784(8) 0.09992(9) 0.12857(6) 0.0274(3) Uani 1.0 4 d .
O1 O 0.1398(5) 0.0463(5) 0.1554(4) 0.0318(14) Uani 1.0 4 d .
O2 O -0.0581(4) 0.0991(5) 0.1677(4) 0.0262(12) Uani 1.0 4 d .
O3 O -0.1794(4) 0.1623(5) 0.0330(4) 0.0285(13) Uani 1.0 4 d .
O4 O -0.0749(5) 0.2342(6) -0.0698(4) 0.0377(15) Uani 1.0 4 d .
O5 O -0.2250(5) -0.0556(5) 0.0823(4) 0.0343(14) Uani 1.0 4 d .
O6 O -0.0678(5) -0.0334(5) 0.0371(4) 0.0327(14) Uani 1.0 4 d .
O7 O -0.1693(5) -0.1729(5) -0.0013(4) 0.0353(14) Uani 1.0 4 d .
O8 O 0.1263(5) 0.2814(6) 0.1354(4) 0.0370(15) Uani 1.0 4 d .
O9 O -0.0433(5) 0.3264(6) 0.0968(4) 0.0365(15) Uani 1.0 4 d .
O10 O 0.0699(6) 0.4380(6) 0.1669(5) 0.0466(18) Uani 1.0 4 d .
O11 O -0.2265(6) 0.2605(6) 0.1706(5) 0.0354(16) Uani 1.0 4 d .
O12 O -0.2132(7) 0.2800(7) 0.3283(5) 0.0432(18) Uani 1.0 4 d .
N1 N -0.2505(6) 0.0400(6) 0.2332(4) 0.0279(15) Uani 1.0 4 d .
N2 N -0.3909(6) 0.1189(7) 0.0775(5) 0.0327(17) Uani 1.0 4 d .
N3 N 0.0530(7) 0.3509(6) 0.1339(5) 0.0341(17) Uani 1.0 4 d .
N4 N -0.1548(17) 0.1353(15) 0.4532(8) 0.142(9) Uani 1.0 4 d .
C1 C 0.2550(7) 0.0401(8) 0.1579(6) 0.035(2) Uani 1.0 4 d .
C2 C 0.0972(7) -0.0067(7) 0.2140(5) 0.0273(18) Uani 1.0 4 d .
C3 C 0.1562(7) -0.0770(8) 0.2670(5) 0.033(2) Uani 1.0 4 d .
C4 C 0.1062(8) -0.1250(8) 0.3235(5) 0.036(2) Uani 1.0 4 d .
C5 C -0.0011(7) -0.0994(8) 0.3266(5) 0.0320(19) Uani 1.0 4 d .
C6 C -0.0620(7) -0.0277(7) 0.2729(5) 0.0273(18) Uani 1.0 4 d .
C7 C -0.0115(7) 0.0237(7) 0.2160(5) 0.0266(18) Uani 1.0 4 d .
C8 C -0.1746(7) -0.0088(7) 0.2813(5) 0.0317(19) Uani 1.0 4 d .
C9 C -0.3580(8) 0.0445(9) 0.2550(6) 0.040(3) Uani 1.0 4 d .
C10 C -0.4498(12) 0.0140(13) 0.1835(9) 0.039(4) Uiso 0.6500 4 d .
C11 C -0.443(3) 0.110(3) 0.2074(16) 0.037(6) Uiso 0.3500 4 d .
C12 C -0.4785(8) 0.0919(10) 0.1205(6) 0.045(3) Uani 1.0 4 d .
C13 C -0.4231(7) 0.1580(8) 0.0083(6) 0.039(3) Uani 1.0 4 d .
C14 C -0.3588(7) 0.1977(8) -0.0467(6) 0.033(2) Uani 1.0 4 d .
C15 C -0.4154(8) 0.2357(8) -0.1195(6) 0.040(3) Uani 1.0 4 d .
C16 C -0.3620(9) 0.2719(9) -0.1760(6) 0.047(3) Uani 1.0 4 d .
C17 C -0.2480(8) 0.2733(8) -0.1622(6) 0.038(2) Uani 1.0 4 d .
C18 C -0.1905(7) 0.2371(7) -0.0903(6) 0.0324(19) Uani 1.0 4 d .
C19 C -0.2417(7) 0.1968(8) -0.0317(5) 0.0320(19) Uani 1.0 4 d .
C20 C -0.0141(9) 0.2835(9) -0.1240(6) 0.042(3) Uani 1.0 4 d .
C21 C -0.1575(8) -0.0868(7) 0.0411(5) 0.0306(19) Uani 1.0 4 d .
C22 C -0.2587(19) -0.0154(14) 0.5175(10) 0.127(9) Uani 1.0 4 d .
C23 C -0.1873(16) 0.0632(14) 0.4808(9) 0.089(5) Uani 1.0 4 d .
H1 H -0.2209 0.2695 0.2055 0.0132 Uiso 1.0 4 calc R
H2 H -0.1686 0.2980 0.1676 0.0738 Uiso 1.0 4 calc R
H3 H -0.2022 0.2305 0.3473 0.0210 Uiso 1.0 4 calc R
H4 H -0.2305 0.3377 0.3661 0.0093 Uiso 1.0 4 calc R
H5 H 0.2758 -0.0349 0.1508 0.0421 Uiso 1.0 4 calc R
H6 H 0.2945 0.0664 0.2090 0.0421 Uiso 1.0 4 calc R
H7 H 0.2743 0.0845 0.1158 0.0421 Uiso 1.0 4 calc R
H8 H 0.2310 -0.0927 0.2651 0.0399 Uiso 1.0 4 calc R
H9 H 0.1459 -0.1752 0.3597 0.0435 Uiso 1.0 4 calc R
H10 H -0.0346 -0.1310 0.3661 0.0384 Uiso 1.0 4 calc R
H11 H -0.1947 -0.0357 0.3279 0.0380 Uiso 1.0 4 calc R
H12 H -0.5008 0.1611 -0.0093 0.0465 Uiso 1.0 4 calc R
H13 H -0.4938 0.2362 -0.1296 0.0479 Uiso 1.0 4 calc R
H14 H -0.4030 0.2961 -0.2250 0.0562 Uiso 1.0 4 calc R
H15 H -0.2098 0.2988 -0.2013 0.0452 Uiso 1.0 4 calc R
H16 H -0.0329 0.2477 -0.1753 0.0509 Uiso 1.0 4 calc R
H17 H 0.0653 0.2763 -0.1035 0.0509 Uiso 1.0 4 calc R
H18 H -0.0334 0.3601 -0.1300 0.0509 Uiso 1.0 4 calc R
H19 H -0.3277 -0.0289 0.4803 0.1524 Uiso 1.0 4 calc R
H20 H -0.2752 0.0159 0.5659 0.1524 Uiso 1.0 4 calc R
H21 H -0.2187 -0.0834 0.5298 0.1524 Uiso 1.0 4 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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Dy Dy -0.1892 4.4098
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Dy1 O2 65.48(19) yes . .
O1 Dy1 O3 133.8(2) yes . .
O1 Dy1 O4 160.9(3) yes . .
O1 Dy1 O6 81.03(19) yes . .
O1 Dy1 O6 87.2(2) yes . 3_555
O1 Dy1 O7 81.9(2) yes . 3_555
O1 Dy1 O8 72.4(2) yes . .
O1 Dy1 O9 113.6(2) yes . .
O1 Dy1 C21 82.9(3) yes . 3_555
O2 Dy1 O3 70.29(19) yes . .
O2 Dy1 O4 133.7(2) yes . .
O2 Dy1 O6 73.3(2) yes . .
O2 Dy1 O6 131.7(2) yes . 3_555
O2 Dy1 O7 144.76(18) yes . 3_555
O2 Dy1 O8 87.1(2) yes . .
O2 Dy1 O9 79.5(2) yes . .
O2 Dy1 C21 145.6(3) yes . 3_555
O3 Dy1 O4 64.6(3) yes . .
O3 Dy1 O6 74.1(2) yes . .
O3 Dy1 O6 113.9(2) yes . 3_555
O3 Dy1 O7 144.1(2) yes . 3_555
O3 Dy1 O8 118.5(2) yes . .
O3 Dy1 O9 69.2(2) yes . .
O3 Dy1 C21 133.9(3) yes . 3_555
O4 Dy1 O6 103.4(2) yes . .
O4 Dy1 O6 78.6(2) yes . 3_555
O4 Dy1 O7 79.5(2) yes . 3_555
O4 Dy1 O8 104.8(2) yes . .
O4 Dy1 O9 75.2(2) yes . .
O4 Dy1 C21 78.6(3) yes . 3_555
O6 Dy1 O6 63.2(3) yes . 3_555
O6 Dy1 O7 116.0(3) yes . 3_555
O6 Dy1 O8 151.8(2) yes . .
O6 Dy1 O9 139.9(2) yes . .
O6 Dy1 C21 89.4(3) yes . 3_555
O6 Dy1 O7 54.7(2) yes 3_555 3_555
O6 Dy1 O8 123.1(2) yes 3_555 .
O6 Dy1 O9 148.6(3) yes 3_555 .
O6 Dy1 C21 27.4(3) yes 3_555 3_555
O7 Dy1 O8 69.9(2) yes 3_555 .
O7 Dy1 O9 103.3(2) yes 3_555 .
O7 Dy1 C21 27.3(3) yes 3_555 3_555
O8 Dy1 O9 50.32(19) yes . .
O8 Dy1 C21 96.3(3) yes . 3_555
O9 Dy1 C21 128.0(3) yes . 3_555
O2 Ni1 O3 80.2(3) yes . .
O2 Ni1 O5 91.7(3) yes . .
O2 Ni1 O11 87.2(3) yes . .
O2 Ni1 N1 90.6(3) yes . .
O2 Ni1 N2 171.0(3) yes . .
O3 Ni1 O5 90.6(3) yes . .
O3 Ni1 O11 86.4(3) yes . .
O3 Ni1 N1 170.7(3) yes . .
O3 Ni1 N2 91.3(3) yes . .
O5 Ni1 O11 176.9(3) yes . .
O5 Ni1 N1 91.1(3) yes . .
O5 Ni1 N2 91.6(3) yes . .
O11 Ni1 N1 91.8(4) yes . .
O11 Ni1 N2 89.0(3) yes . .
N1 Ni1 N2 97.8(3) yes . .
Dy1 O1 C1 125.4(6) yes . .
Dy1 O1 C2 116.6(5) yes . .
C1 O1 C2 118.0(7) yes . .
Dy1 O2 Ni1 102.4(2) yes . .
Dy1 O2 C7 121.2(5) yes . .
Ni1 O2 C7 120.3(5) yes . .
Dy1 O3 Ni1 105.5(3) yes . .
Dy1 O3 C19 126.3(6) yes . .
Ni1 O3 C19 127.7(6) yes . .
Dy1 O4 C18 117.1(6) yes . .
Dy1 O4 C20 125.9(5) yes . .
C18 O4 C20 117.0(7) yes . .
Ni1 O5 C21 124.3(6) yes . .
Dy1 O6 Dy1 116.8(3) yes . 3_555
Dy1 O6 C21 141.0(6) yes . .
Dy1 O6 C21 97.8(5) yes 3_555 .
Dy1 O7 C21 94.1(6) yes 3_555 .
Dy1 O8 N3 97.0(5) yes . .
Dy1 O9 N3 96.1(5) yes . .
Ni1 N1 C8 123.0(7) yes . .
Ni1 N1 C9 120.6(6) yes . .
C8 N1 C9 116.2(8) yes . .
Ni1 N2 C12 121.0(6) yes . .
Ni1 N2 C13 123.3(7) yes . .
C12 N2 C13 115.7(8) yes . .
O8 N3 O9 116.6(7) yes . .
O8 N3 O10 122.9(8) yes . .
O9 N3 O10 120.4(8) yes . .
O1 C2 C3 124.1(8) yes . .
O1 C2 C7 112.9(7) yes . .
C3 C2 C7 122.9(8) yes . .
C2 C3 C4 119.6(9) yes . .
C3 C4 C5 119.4(8) yes . .
C4 C5 C6 121.4(9) yes . .
C5 C6 C7 119.8(8) yes . .
C5 C6 C8 116.2(8) yes . .
C7 C6 C8 123.9(8) yes . .
O2 C7 C2 118.8(8) yes . .
O2 C7 C6 124.5(8) yes . .
C2 C7 C6 116.7(8) yes . .
N1 C8 C6 127.6(9) yes . .
N1 C9 C10 110.3(9) yes . .
N1 C9 C11 118.2(14) yes . .
C10 C9 C11 49.3(13) yes . .
C9 C10 C11 61.1(14) yes . .
C9 C10 C12 118.1(12) yes . .
C11 C10 C12 66.8(15) yes . .
C9 C11 C10 69.6(16) yes . .
C9 C11 C12 122(2) yes . .
C10 C11 C12 62.7(15) yes . .
N2 C12 C10 115.9(10) yes . .
N2 C12 C11 112.1(13) yes . .
C10 C12 C11 50.4(13) yes . .
N2 C13 C14 129.5(8) yes . .
C13 C14 C15 117.9(8) yes . .
C13 C14 C19 123.3(8) yes . .
C15 C14 C19 118.9(9) yes . .
C14 C15 C16 122.2(9) yes . .
C15 C16 C17 120.0(9) yes . .
C16 C17 C18 118.7(10) yes . .
O4 C18 C17 123.9(9) yes . .
O4 C18 C19 112.9(7) yes . .
C17 C18 C19 123.2(8) yes . .
O3 C19 C14 124.9(9) yes . .
O3 C19 C18 118.1(8) yes . .
C14 C19 C18 117.0(8) yes . .
Dy1 C21 O5 175.8(7) yes 3_555 .
Dy1 C21 O6 54.8(5) yes 3_555 .
Dy1 C21 O7 58.6(5) yes 3_555 .
O5 C21 O6 122.3(8) yes . .
O5 C21 O7 124.4(9) yes . .
O6 C21 O7 113.3(9) yes . .
N4 C23 C22 165(2) yes . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Dy1 O1 2.451(6) yes .
Dy1 O2 2.309(6) yes .
Dy1 O3 2.273(5) yes .
Dy1 O4 2.487(6) yes .
Dy1 O6 2.349(6) yes .
Dy1 O6 2.312(7) yes 3_555
Dy1 O7 2.398(7) yes 3_555
Dy1 O8 2.524(6) yes .
Dy1 O9 2.526(7) yes .
Dy1 C21 2.803(10) yes 3_555
Ni1 O2 2.074(5) yes .
Ni1 O3 2.019(7) yes .
Ni1 O5 2.092(7) yes .
Ni1 O11 2.120(8) yes .
Ni1 N1 2.028(8) yes .
Ni1 N2 2.050(7) yes .
O1 C1 1.416(10) yes .
O1 C2 1.393(11) yes .
O2 C7 1.313(10) yes .
O3 C19 1.304(10) yes .
O4 C18 1.403(11) yes .
O4 C20 1.446(13) yes .
O5 C21 1.257(12) yes .
O6 C21 1.303(11) yes .
O7 C21 1.289(11) yes .
O8 N3 1.248(10) yes .
O9 N3 1.275(9) yes .
O10 N3 1.222(11) yes .
N1 C8 1.280(11) yes .
N1 C9 1.449(12) yes .
N2 C12 1.464(14) yes .
N2 C13 1.285(13) yes .
N4 C23 1.12(3) yes .
C2 C3 1.371(12) yes .
C2 C7 1.400(12) yes .
C3 C4 1.387(14) yes .
C4 C5 1.373(14) yes .
C5 C6 1.398(12) yes .
C6 C7 1.415(13) yes .
C6 C8 1.444(13) yes .
C9 C10 1.556(16) yes .
C9 C11 1.45(3) yes .
C10 C11 1.26(4) yes .
C10 C12 1.451(18) yes .
C11 C12 1.50(3) yes .
C13 C14 1.438(15) yes .
C14 C15 1.401(13) yes .
C14 C19 1.418(12) yes .
C15 C16 1.356(16) yes .
C16 C17 1.383(15) yes .
C17 C18 1.384(12) yes .
C18 C19 1.389(14) yes .
C22 C23 1.53(3) yes .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O11 H1 O12 2_645 2.712(8) 0.820 1.957 152.9 no
O11 H2 O9 . 2.917(8) 0.962 1.997 159.3 no
O12 H3 N3 . 2.839(14) 0.843 2.102 145.8 no
O12 H4 O5 1_565 2.762(8) 1.042 1.748 163.2 no
