Series of Trinuclear NiIILnIIINiII Complexes Derived from 2,6-Di(acetoacetyl)pyridine: Synthesis, Structure, and Magnetism
Takuya Shiga; Nobuhiro Ito; Akiko Hidaka; Hisashi Ōkawa; Susumu Kitagawa; Masaaki Ohba; Inorganic Chemistry 46 (2007) 3492–3501; doi:10.1021/ic0619153

data_4307433
_publ_contact_author_address
;Department of Synthetic Chemistry and Biological Chemistry,
Graduate School of Engineering,
Kyoto University,
Katsura, Nishikyo-ku, Kyoto 615-8510, Japan
;
_publ_contact_author_email       ohba@sbchem.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-383-2732
_publ_contact_author_name        'Masaaki Ohba'
_publ_contact_author_phone       +81-75-383-2807
_publ_section_title
;
Series of Trinuclear NiIILnIIINiII Complexes Derived from
2,6-Di(acetoacetyl)pyridine: Synthesis, Structure, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3492
_journal_page_last               3501
_journal_paper_doi               10.1021/ic0619153
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C31 H42 Eu N5 Ni2 O22'
_chemical_formula_weight         1106.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                92.424(2)
_cell_angle_beta                 104.477(4)
_cell_angle_gamma                91.207(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7920(6)
_cell_length_b                   9.3695(8)
_cell_length_c                   14.451(1)
_cell_measurement_reflns_used    5596
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.5
_cell_volume                     1020.07(14)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 8.00
_diffrn_measured_fraction_theta_full 0.9876
_diffrn_measured_fraction_theta_max 0.9876
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9377
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_exptl_absorpt_coefficient_mu    2.520
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4530
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.06300(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                4270
_reflns_number_total             1513
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_06.cif
_cod_data_source_block           6-A_Ni2Eu_A_[Ni2Eu(L)2(NO3)2(MeOH)4]NO3.MeOH
_cod_depositor_comments
;

  Following atoms were removed leaving only those belonging to
  asymmetric unit:

  O(2*) O -0.1024(3) -0.0686(2) -0.1770(1) 0.0200(4) Uani 1.00 d . . .
  O(3*) O 0.1766(3) -0.1756(2) 0.1081(1) 0.0202(4) Uani 1.00 d . . .
  O(5*) O -0.2306(3) -0.1960(2) -0.0152(2) 0.0395(7) Uani 1.00 d . . .
  O(6*) O -0.2683(3) -0.0087(2) 0.0646(2) 0.0376(6) Uani 1.00 d . . .
  N(1*) N 0.0801(3) -0.2568(2) -0.0705(2) 0.0176(5) Uani 1.00 d . . .
  N(2*) N -0.3165(3) -0.1359(3) 0.0361(2) 0.0252(6) Uani 1.00 d . . .
  O(4*) O 0.3918(3) -0.2479(2) 0.2978(1) 0.0341(6) Uani 1.00 d . . .
  Ni(*) Ni -0.25118(5) 0.08656(3) -0.24131(2) 0.02057(9) Uani 1.00 d . . .
  O(9*) O -0.1168(9) 0.4351(8) 0.4366(4) 0.064(2) Uani 0.50 d P . .
  O(13*) O 0.127(2) 0.647(1) 0.4284(7) 0.076(3) Uani 0.50 d P . .
  H(20*) H 0.0944 0.5385 0.4333 0.0295 Uiso 0.50 calc P . .
  O(8*) O 0.033(1) 0.4480(8) 0.5795(4) 0.077(2) Uani 0.50 d P . .
  C(16*) C 0.213(2) 0.734(2) 0.5136(10) 0.080(4) Uani 0.50 d P . .
  H(23*) H 0.2113 0.8263 0.4952 0.0888 Uiso 0.50 calc P . .
  O(10*) O -0.179(2) 0.297(2) 0.5336(9) 0.118(7) Uani 0.50 d P . .
  N(3*) N -0.0935(9) 0.3940(8) 0.5178(4) 0.046(2) Uani 0.50 d P . .
  C(4*) C -0.0773(3) -0.1837(3) -0.2242(2) 0.0198(6) Uani 1.00 d . . .
  C(10*) C 0.2218(3) -0.3041(3) 0.0905(2) 0.0176(6) Uani 1.00 d . . .
  C(5*) C 0.0346(4) -0.2898(3) -0.1653(2) 0.0205(6) Uani 1.00 d . . .
  C(9*) C 0.1754(4) -0.3492(3) -0.0130(2) 0.0194(6) Uani 1.00 d . . .
  O(7*) O -0.4394(3) -0.1967(3) 0.0591(2) 0.0430(7) Uani 1.00 d . . .
  C(12*) C 0.3886(4) -0.3665(3) 0.2550(2) 0.0275(7) Uani 1.00 d . . .
  O(1*) O -0.3237(3) -0.0161(2) -0.3682(1) 0.0322(5) Uani 1.00 d . . .
  O(11*) O -0.4717(3) 0.0001(3) -0.2013(2) 0.0440(7) Uani 1.00 d . . .
  O(12*) O -0.0424(3) 0.1910(3) -0.2818(2) 0.0362(6) Uani 1.00 d . . .
  H(21*) H 0.1417 0.7244 0.5606 0.0888 Uiso 0.50 calc P . .
  H(22*) H 0.3210 0.6965 0.5358 0.0888 Uiso 0.50 calc P . .
  C(3*) C -0.1460(4) -0.2151(3) -0.3212(2) 0.0303(7) Uani 1.00 d . . .
  C(11*) C 0.3074(4) -0.3968(3) 0.1564(2) 0.0246(7) Uani 1.00 d . . .
  C(6*) C 0.0870(5) -0.4155(3) -0.2040(2) 0.0314(8) Uani 1.00 d . . .
  C(8*) C 0.2339(4) -0.4764(3) -0.0470(2) 0.0285(7) Uani 1.00 d . . .
  C(13*) C 0.4810(6) -0.4850(4) 0.3136(2) 0.0448(10) Uani 1.00 d . . .
  C(2*) C -0.2640(4) -0.1325(3) -0.3881(2) 0.0313(8) Uani 1.00 d . . .
  C(14*) C -0.5444(5) -0.1406(4) -0.2225(3) 0.048(1) Uani 1.00 d . . .
  H(12*) H -0.4922 0.0414 -0.1514 0.0295 Uiso 1.00 calc . . .
  C(15*) C 0.1094(5) 0.1251(5) -0.2982(3) 0.049(1) Uani 1.00 d . . .
  H(16*) H -0.0807 0.2408 -0.3353 0.0295 Uiso 1.00 calc . . .
  H(4*) H -0.1141 -0.3072 -0.3504 0.0295 Uiso 1.00 calc . . .
  H(8*) H 0.3235 -0.4944 0.1395 0.0295 Uiso 1.00 calc . . .
  C(7*) C 0.1887(5) -0.5079(3) -0.1439(2) 0.0364(8) Uani 1.00 d . . .
  H(5*) H 0.0407 -0.4523 -0.2609 0.0295 Uiso 1.00 calc . . .
  H(7*) H 0.3127 -0.5372 -0.0181 0.0295 Uiso 1.00 calc . . .
  H(9*) H 0.5610 -0.5287 0.2814 0.0516 Uiso 1.00 calc . . .
  H(10*) H 0.3970 -0.5541 0.3219 0.0516 Uiso 1.00 calc . . .
  H(11*) H 0.5468 -0.4460 0.3743 0.0516 Uiso 1.00 calc . . .
  C(1*) C -0.3239(7) -0.1906(5) -0.4884(2) 0.068(1) Uani 1.00 d . . .
  H(13*) H -0.5497 -0.1673 -0.2916 0.0295 Uiso 0.50 calc P . .
  H(13'*) H -0.4586 -0.2010 -0.2404 0.0588 Uiso 0.50 calc P . .
  H(14*) H -0.6575 -0.1408 -0.2126 0.0295 Uiso 0.50 calc P . .
  H(14'*) H -0.6469 -0.1416 -0.2753 0.0588 Uiso 0.50 calc P . .
  H(15*) H -0.4580 -0.2085 -0.1854 0.0295 Uiso 0.50 calc P . .
  H(15'*) H -0.5751 -0.1762 -0.1688 0.0588 Uiso 0.50 calc P . .
  H(17*) H 0.1588 0.0685 -0.2469 0.0574 Uiso 1.00 calc . . .
  H(18*) H 0.0737 0.0661 -0.3562 0.0574 Uiso 1.00 calc . . .
  H(19*) H 0.1918 0.1962 -0.3058 0.0574 Uiso 1.00 calc . . .
  H(6*) H 0.2206 -0.5980 -0.1686 0.0295 Uiso 1.00 calc . . .
  H(1*) H -0.4187 -0.1359 -0.5228 0.0801 Uiso 1.00 calc . . .
  H(2*) H -0.2307 -0.1914 -0.5183 0.0801 Uiso 1.00 calc . . .
  H(3*) H -0.3701 -0.2880 -0.4887 0.0801 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_cell_volume        1020.1(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H42 Eu N5 O22 Ni2 '
_cod_database_code               4307433