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_4307434
_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 H38 Gd N5 Ni2 O22'
_chemical_formula_weight         1107.31
_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                92.321(3)
_cell_angle_beta                 104.321(3)
_cell_angle_gamma                91.211(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8220(4)
_cell_length_b                   9.3686(5)
_cell_length_c                   14.4871(9)
_cell_measurement_reflns_used    9249
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.7
_cell_volume                     1027.27(10)
_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 0.9707
_diffrn_measured_fraction_theta_max 0.9707
_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  0.027
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9008
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    2.597
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4536
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.0052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.07200(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                4146
_reflns_number_total             4542
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_07.cif
_cod_data_source_block           7-A_Ni2Gd_A_[Ni2Gd(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 -0.1027(3) -0.0689(3) -0.1770(2) 0.0239(6) Uani 1.00 d . . .
  O(3*) O 0.1772(3) -0.1741(3) 0.1085(2) 0.0238(6) Uani 1.00 d . . .
  O(5*) O -0.2292(4) -0.1956(3) -0.0143(3) 0.049(1) Uani 1.00 d . . .
  O(6*) O -0.2664(4) -0.0091(4) 0.0653(3) 0.0448(9) Uani 1.00 d . . .
  N(1*) N 0.0804(4) -0.2565(3) -0.0705(2) 0.0201(7) Uani 1.00 d . . .
  O(4*) O 0.3920(4) -0.2478(3) 0.2976(2) 0.0418(8) Uani 1.00 d . . .
  Ni(*) Ni -0.25170(6) 0.08573(5) -0.24124(3) 0.0245(1) Uani 1.00 d . . .
  O(9*) O 0.882(1) 0.435(1) 0.4364(6) 0.072(3) Uani 0.50 d P . .
  O(13*) O 1.130(2) 0.650(1) 0.4281(8) 0.076(4) Uani 0.50 d P . .
  O(8*) O 1.032(2) 0.449(1) 0.5799(6) 0.088(3) Uani 0.50 d P . .
  C(16*) C 1.218(3) 0.738(3) 0.519(2) 0.098(7) Uani 0.50 d P . .
  O(10*) O 0.817(2) 0.295(2) 0.531(1) 0.123(8) Uani 0.50 d P . .
  N(3*) N 0.906(1) 0.396(1) 0.5200(7) 0.054(3) Uani 0.50 d P . .
  C(4*) C -0.0791(5) -0.1841(4) -0.2239(3) 0.0244(9) Uani 1.00 d . . .
  C(10*) C 0.2223(4) -0.3025(4) 0.0908(2) 0.0209(8) Uani 1.00 d . . .
  N(2*) N -0.3151(4) -0.1353(4) 0.0361(3) 0.0289(8) Uani 1.00 d . . .
  C(5*) C 0.0339(5) -0.2910(4) -0.1651(3) 0.0231(8) Uani 1.00 d . . .
  C(9*) C 0.1769(5) -0.3495(4) -0.0123(3) 0.0215(8) Uani 1.00 d . . .
  C(12*) C 0.3896(5) -0.3658(4) 0.2551(3) 0.0312(10) Uani 1.00 d . . .
  O(1*) O -0.3240(4) -0.0168(3) -0.3677(2) 0.0374(8) Uani 1.00 d . . .
  O(11*) O -0.4724(4) -0.0001(4) -0.2011(3) 0.050(1) Uani 1.00 d . . .
  O(12*) O -0.0432(4) 0.1903(4) -0.2817(2) 0.0397(8) Uani 1.00 d . . .
  C(3*) C -0.1464(6) -0.2167(5) -0.3203(3) 0.036(1) Uani 1.00 d . . .
  C(11*) C 0.3088(5) -0.3960(4) 0.1564(3) 0.0279(9) Uani 1.00 d . . .
  O(7*) O -0.4383(4) -0.1964(4) 0.0592(3) 0.050(1) Uani 1.00 d . . .
  C(6*) C 0.0866(6) -0.4156(4) -0.2036(3) 0.034(1) Uani 1.00 d . . .
  C(8*) C 0.2338(6) -0.4765(4) -0.0470(3) 0.033(1) Uani 1.00 d . . .
  C(13*) C 0.4843(8) -0.4839(5) 0.3132(3) 0.048(1) Uani 1.00 d . . .
  C(2*) C -0.2642(6) -0.1324(5) -0.3874(3) 0.034(1) Uani 1.00 d . . .
  C(14*) C -0.5444(7) -0.1420(6) -0.2215(5) 0.057(2) Uani 1.00 d . . .
  H(12*) H -0.5300 0.0627 -0.1658 0.0600 Uiso 1.00 calc . . .
  C(15*) C 0.1083(7) 0.1249(7) -0.2985(4) 0.057(2) Uani 1.00 d . . .
  H(16*) H -0.0526 0.2914 -0.2900 0.0478 Uiso 1.00 calc . . .
  H(4*) H -0.0868 -0.3037 -0.3531 0.0329 Uiso 1.00 calc . . .
  H(8*) H 0.3285 -0.4780 0.1318 0.0329 Uiso 1.00 calc . . .
  C(7*) C 0.1866(7) -0.5084(4) -0.1441(3) 0.039(1) Uani 1.00 d . . .
  H(5*) H 0.0704 -0.4227 -0.2680 0.0556 Uiso 1.00 calc . . .
  H(7*) H 0.3070 -0.5283 -0.0030 0.0501 Uiso 1.00 calc . . .
  H(9*) H 0.3992 -0.5463 0.3295 0.0575 Uiso 1.00 calc . . .
  H(10*) H 0.5496 -0.5354 0.2773 0.0575 Uiso 1.00 calc . . .
  H(11*) H 0.5607 -0.4434 0.3702 0.0575 Uiso 1.00 calc . . .
  C(1*) C -0.3235(10) -0.1915(7) -0.4885(4) 0.071(2) Uani 1.00 d . . .
  H(13*) H -0.4577 -0.2070 -0.1960 0.0698 Uiso 1.00 calc . . .
  H(14*) H -0.6432 -0.1523 -0.1953 0.0698 Uiso 1.00 calc . . .
  H(15*) H -0.5821 -0.1579 -0.2894 0.0698 Uiso 1.00 calc . . .
  H(17*) H 0.0740 0.0534 -0.3482 0.0688 Uiso 1.00 calc . . .
  H(18*) H 0.1832 0.1948 -0.3160 0.0688 Uiso 1.00 calc . . .
  H(19*) H 0.1707 0.0828 -0.2417 0.0688 Uiso 1.00 calc . . .
  H(6*) H 0.2227 -0.5940 -0.1694 0.0461 Uiso 1.00 calc . . .
  H(1*) H -0.2350 -0.1746 -0.5209 0.0864 Uiso 1.00 calc . . .
  H(2*) H -0.4289 -0.1446 -0.5202 0.0864 Uiso 1.00 calc . . .
  H(3*) H -0.3498 -0.2907 -0.4892 0.0864 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_cell_volume        1027.26(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H38 Gd N5 O22 Ni2 '
_cod_database_code               4307434