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_4307441
_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_moiety         'C30 H36 Dy N5 O21 Ni2 '
_chemical_formula_sum            'C30 H36 Dy N5 Ni2 O21'
_chemical_formula_weight         1082.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 99.187(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0708(6)
_cell_length_b                   17.2309(9)
_cell_length_c                   16.2927(9)
_cell_measurement_reflns_used    18520
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.3
_cell_volume                     3899.5(3)
_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    DirectMethod
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9937
_diffrn_measured_fraction_theta_max 0.9937
_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  0.033
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16553
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_exptl_absorpt_coefficient_mu    2.946
_exptl_absorpt_correction_T_max  0.290
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.420
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4421
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.0073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.08800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                4055
_reflns_number_total             4423
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_14.cif
_cod_data_source_block           9_Ni2Dy_C_[Ni2Dy(L)2(NO3)3(MeOH)4]
_cod_depositor_comments
;

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

  O(2*) O -0.1718(2) 0.1438(1) 0.2008(1) 0.0243(5) Uani 1.00 d . . .
  O(3*) O 0.1108(1) 0.0881(1) 0.1517(1) 0.0231(5) Uani 1.00 d . . .
  O(5*) O 0.0419(2) 0.2405(1) 0.1759(1) 0.0306(6) Uani 1.00 d . . .
  O(8*) O -0.0673(2) -0.0062(1) 0.2073(1) 0.0285(6) Uani 1.00 d . . .
  N(1*) N -0.0655(2) 0.1188(2) 0.0880(2) 0.0206(6) Uani 1.00 d . . .
  O(4*) O 0.3070(2) 0.0732(2) 0.1163(1) 0.0317(6) Uani 1.00 d . . .
  Ni(*) Ni -0.24486(3) 0.11452(3) 0.29219(3) 0.0244(1) Uani 1.00 d . . .
  C(4*) C -0.2182(2) 0.1498(2) 0.1254(2) 0.0228(7) Uani 1.00 d . . .
  C(10*) C 0.0951(2) 0.0848(2) 0.0713(2) 0.0220(7) Uani 1.00 d . . .
  N(2*) N -0.0105(2) 0.2935(2) 0.1348(2) 0.0274(7) Uani 1.00 d . . .
  C(5*) C -0.1568(2) 0.1395(2) 0.0593(2) 0.0232(7) Uani 1.00 d . . .
  C(9*) C -0.0061(2) 0.1044(2) 0.0331(2) 0.0231(7) Uani 1.00 d . . .
  C(12*) C 0.2628(2) 0.0578(2) 0.0455(2) 0.0269(8) Uani 1.00 d . . .
  O(1*) O -0.3711(2) 0.1482(2) 0.2321(1) 0.0358(8) Uani 1.00 d . . .
  O(10*) O -0.2247(2) 0.2243(2) 0.3468(2) 0.0412(7) Uani 1.00 d . . .
  O(11*) O -0.2643(2) 0.0048(2) 0.2359(2) 0.0400(7) Uani 1.00 d . . .
  C(3*) C -0.3151(2) 0.1623(2) 0.1026(2) 0.0273(8) Uani 1.00 d . . .
  C(11*) C 0.1616(2) 0.0667(2) 0.0202(2) 0.0257(8) Uani 1.00 d . . .
  O(6*) O -0.0968(2) 0.2959(2) 0.1361(2) 0.0429(7) Uani 1.00 d . . .
  O(7*) O 0.0304(2) 0.3396(2) 0.0950(2) 0.0585(10) Uani 1.00 d . . .
  C(6*) C -0.1905(2) 0.1483(2) -0.0253(2) 0.0292(8) Uani 1.00 d . . .
  C(8*) C -0.0349(3) 0.1110(2) -0.0523(2) 0.0317(9) Uani 1.00 d . . .
  C(13*) C 0.3232(3) 0.0300(2) -0.0166(2) 0.0344(9) Uani 1.00 d . . .
  C(2*) C -0.3858(2) 0.1642(2) 0.1563(2) 0.0314(9) Uani 1.00 d . . .
  C(14*) C -0.2846(7) 0.2869(6) 0.335(1) 0.069(3) Uani 0.50 d P . .
  C(14'*) C -0.2667(9) 0.2649(8) 0.403(1) 0.091(5) Uani 0.50 d P . .
  H(12*) H -0.1663 0.2363 0.3554 0.0359 Uiso 1.00 calc . . .
  C(15*) C -0.3387(4) -0.0471(3) 0.2451(3) 0.063(2) Uani 1.00 d . . .
  H(15*) H -0.2100 -0.0192 0.2238 0.0359 Uiso 1.00 calc . . .
  H(4*) H -0.3461 0.1693 0.0499 0.0359 Uiso 1.00 calc . . .
  H(8*) H 0.1373 0.0631 -0.0372 0.0359 Uiso 1.00 calc . . .
  C(7*) C -0.1293(3) 0.1338(2) -0.0816(2) 0.0353(10) Uani 1.00 d . . .
  H(5*) H -0.2513 0.1595 -0.0453 0.0359 Uiso 1.00 calc . . .
  H(7*) H 0.0039 0.1047 -0.0901 0.0359 Uiso 1.00 calc . . .
  H(9*) H 0.2872 0.0166 -0.0667 0.0359 Uiso 1.00 calc . . .
  H(10*) H 0.3574 -0.0122 0.0040 0.0359 Uiso 1.00 calc . . .
  H(11*) H 0.3775 0.0613 -0.0212 0.0359 Uiso 1.00 calc . . .
  C(1*) C -0.4874(2) 0.1836(3) 0.1198(3) 0.045(1) Uani 1.00 d . . .
  H(13*) H -0.2626 0.3353 0.3215 0.0855 Uiso 0.50 calc P . .
  H(14*) H -0.3499 0.2791 0.3081 0.0855 Uiso 0.50 calc P . .
  H(13'*) H -0.2278 0.2978 0.4384 0.0921 Uiso 0.50 calc P . .
  H(14'*) H -0.3151 0.2417 0.4251 0.0921 Uiso 0.50 calc P . .
  H(16*) H -0.3290 -0.0776 0.2974 0.0359 Uiso 1.00 calc . . .
  H(17*) H -0.3381 -0.0915 0.2205 0.0359 Uiso 1.00 calc . . .
  H(18*) H -0.3936 -0.0231 0.2337 0.0359 Uiso 1.00 calc . . .
  H(6*) H -0.1507 0.1326 -0.1391 0.0359 Uiso 1.00 calc . . .
  H(1*) H -0.4908 0.2025 0.0672 0.0359 Uiso 1.00 calc . . .
  H(2*) H -0.5106 0.2311 0.1424 0.0359 Uiso 1.00 calc . . .
  H(3*) H -0.5323 0.1629 0.1443 0.0359 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_formula_sum        'C30 H36 Dy N5 O21 Ni2 '
_cod_database_code               4307441