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_4307428
_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 La N5 Ni2 O22'
_chemical_formula_weight         1093.00
_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                92.775(2)
_cell_angle_beta                 104.760(2)
_cell_angle_gamma                91.309(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8700(4)
_cell_length_b                   9.4406(4)
_cell_length_c                   14.5086(5)
_cell_measurement_reflns_used    5497
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     1040.47(8)
_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 0.9886
_diffrn_measured_fraction_theta_max 0.9886
_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  0.026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9859
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4695
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.08600(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                4379
_reflns_number_total             4697
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_01.cif
_cod_data_source_block           1_Ni2La_A_[Ni2La(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 -0.1014(3) -0.0696(2) -0.1800(1) 0.0261(4) Uani 1.00 d . . .
  O(3*) O 0.1760(3) -0.1803(2) 0.1088(1) 0.0259(4) Uani 1.00 d . . .
  O(5*) O -0.2432(3) -0.1995(2) -0.0156(2) 0.0437(6) Uani 1.00 d . . .
  O(6*) O -0.2803(3) -0.0120(2) 0.0657(2) 0.0409(6) Uani 1.00 d . . .
  N(1*) N 0.0779(3) -0.2592(2) -0.0728(2) 0.0222(5) Uani 1.00 d . . .
  O(4*) O 0.3858(3) -0.2515(2) 0.2957(2) 0.0440(6) Uani 1.00 d . . .
  Ni(1*) Ni -0.24792(5) 0.08851(4) -0.24158(2) 0.02666(10) Uani 1.00 d . . .
  O(9*) O -0.126(1) 0.4343(10) 0.4391(5) 0.087(3) Uani 0.50 d P . .
  O(13*) O 0.112(2) 0.643(1) 0.4241(7) 0.087(3) Uani 0.50 d P . .
  H(20*) H 0.0421 0.5422 0.4256 0.0341 Uiso 0.50 calc P . .
  O(8*) O 0.046(2) 0.440(1) 0.5788(5) 0.108(3) Uani 0.50 d P . .
  C(16*) C 0.204(2) 0.732(1) 0.5119(9) 0.079(4) Uani 0.50 d P . .
  O(10*) O -0.175(2) 0.307(2) 0.541(1) 0.160(7) Uani 0.50 d P . .
  N(3*) N -0.0937(9) 0.3942(8) 0.5214(6) 0.058(2) Uani 0.50 d P . .
  C(4*) C -0.0791(3) -0.1853(3) -0.2271(2) 0.0248(6) Uani 1.00 d . . .
  C(10*) C 0.2195(3) -0.3080(3) 0.0892(2) 0.0228(6) Uani 1.00 d . . .
  N(2*) N -0.3264(3) -0.1393(3) 0.0380(2) 0.0332(6) Uani 1.00 d . . .
  C(5*) C 0.0327(3) -0.2916(3) -0.1673(2) 0.0252(6) Uani 1.00 d . . .
  C(9*) C 0.1728(3) -0.3519(3) -0.0151(2) 0.0230(6) Uani 1.00 d . . .
  C(12*) C 0.3857(4) -0.3688(3) 0.2529(2) 0.0340(7) Uani 1.00 d . . .
  O(1*) O -0.3199(3) -0.0151(3) -0.3684(2) 0.0412(6) Uani 1.00 d . . .
  O(11*) O -0.4654(4) 0.0020(3) -0.2016(2) 0.0556(8) Uani 1.00 d . . .
  O(12*) O -0.0385(3) 0.1910(3) -0.2805(2) 0.0420(6) Uani 1.00 d . . .
  H(21*) H 0.2508 0.8176 0.4902 0.1044 Uiso 0.50 calc P . .
  H(22*) H 0.2858 0.6855 0.5510 0.1044 Uiso 0.50 calc P . .
  H(23*) H 0.1122 0.7649 0.5412 0.1044 Uiso 0.50 calc P . .
  C(3*) C -0.1469(5) -0.2161(3) -0.3230(2) 0.0378(8) Uani 1.00 d . . .
  C(11*) C 0.3066(4) -0.4006(3) 0.1547(2) 0.0297(7) Uani 1.00 d . . .
  O(7*) O -0.4427(3) -0.2019(3) 0.0630(2) 0.0557(8) Uani 1.00 d . . .
  C(6*) C 0.0854(4) -0.4145(3) -0.2070(2) 0.0369(7) Uani 1.00 d . . .
  C(8*) C 0.2311(4) -0.4768(3) -0.0500(2) 0.0351(7) Uani 1.00 d . . .
  C(13*) C 0.4792(6) -0.4859(4) 0.3113(3) 0.0515(10) Uani 1.00 d . . .
  C(2*) C -0.2636(5) -0.1318(4) -0.3893(2) 0.0406(8) Uani 1.00 d . . .
  C(14*) C -0.5429(5) -0.1349(4) -0.2248(4) 0.061(1) Uani 1.00 d . . .
  H(16*) H -0.5006 0.0495 -0.1567 0.0341 Uiso 1.00 calc . . .
  C(15*) C 0.1089(6) 0.1234(5) -0.2985(3) 0.061(1) Uani 1.00 d . . .
  H(12*) H -0.0901 0.2393 -0.3334 0.0341 Uiso 1.00 calc . . .
  H(4*) H -0.1513 -0.3243 -0.3517 0.0341 Uiso 1.00 calc . . .
  H(8*) H 0.3295 -0.4938 0.1338 0.0341 Uiso 1.00 calc . . .
  C(7*) C 0.1849(5) -0.5080(3) -0.1469(2) 0.0429(8) Uani 1.00 d . . .
  H(5*) H 0.0745 -0.4386 -0.2721 0.0341 Uiso 1.00 calc . . .
  H(7*) H 0.2926 -0.5614 -0.0143 0.0341 Uiso 1.00 calc . . .
  H(9*) H 0.4231 -0.5756 0.2871 0.0341 Uiso 1.00 calc . . .
  H(10*) H 0.5873 -0.4421 0.3361 0.0341 Uiso 1.00 calc . . .
  H(11*) H 0.4223 -0.4773 0.3580 0.0341 Uiso 1.00 calc . . .
  C(1*) C -0.3214(8) -0.1855(6) -0.4922(3) 0.080(1) Uani 1.00 d . . .
  H(17*) H -0.6328 -0.1491 -0.1927 0.0723 Uiso 1.00 calc . . .
  H(18*) H -0.4549 -0.2049 -0.2038 0.0723 Uiso 1.00 calc . . .
  H(19*) H -0.5896 -0.1498 -0.2912 0.0723 Uiso 1.00 calc . . .
  H(13*) H 0.1606 0.0673 -0.2467 0.0734 Uiso 1.00 calc . . .
  H(14*) H 0.1914 0.1913 -0.3076 0.0734 Uiso 1.00 calc . . .
  H(15*) H 0.0707 0.0618 -0.3553 0.0734 Uiso 1.00 calc . . .
  H(6*) H 0.2119 -0.5981 -0.1738 0.0341 Uiso 1.00 calc . . .
  H(1*) H -0.3814 -0.1102 -0.5284 0.0341 Uiso 1.00 calc . . .
  H(2*) H -0.4175 -0.2479 -0.4655 0.0341 Uiso 1.00 calc . . .
  H(3*) H -0.2578 -0.2454 -0.5091 0.0341 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H42 La N5 O22 Ni2 '
_cod_database_code               4307428