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_4307440
_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 H38 N5 O21 Ni2 Tb '
_chemical_formula_sum            'C30 H38 N5 Ni2 O21 Tb'
_chemical_formula_weight         1080.98
_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                 99.2495(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1121(5)
_cell_length_b                   17.2313(6)
_cell_length_c                   16.3004(6)
_cell_measurement_reflns_used    19920
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.3
_cell_volume                     3912.2(2)
_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 5.00
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9959
_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       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17211
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.57
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4394
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.06400(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                3707
_reflns_number_total             4397
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_13.cif
_cod_data_source_block           8_Ni2Tb_C_[Ni2Tb(L)2(NO3)3(MeOH)4]
_cod_depositor_comments
;

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

  O(2*) O -0.1720(2) 0.1432(2) 0.2006(2) 0.0242(6) Uani 1.00 d . . .
  O(3*) O 0.1104(2) 0.0885(2) 0.1513(1) 0.0221(6) Uani 1.00 d . . .
  O(5*) O 0.0413(2) 0.2413(2) 0.1763(2) 0.0325(8) Uani 1.00 d . . .
  O(8*) O -0.0671(2) -0.0074(2) 0.2078(2) 0.0300(7) Uani 1.00 d . . .
  N(1*) N -0.0661(2) 0.1186(2) 0.0879(2) 0.0205(7) Uani 1.00 d . . .
  O(4*) O 0.3065(2) 0.0736(2) 0.1158(2) 0.0330(8) Uani 1.00 d . . .
  Ni(*) Ni -0.24468(3) 0.11431(3) 0.29227(3) 0.0247(1) Uani 1.00 d . . .
  C(4*) C -0.2185(3) 0.1494(2) 0.1253(2) 0.0222(8) Uani 1.00 d . . .
  C(10*) C 0.0945(3) 0.0851(2) 0.0706(2) 0.0217(9) Uani 1.00 d . . .
  N(2*) N -0.0103(3) 0.2942(2) 0.1347(2) 0.0304(9) Uani 1.00 d . . .
  C(5*) C -0.1569(3) 0.1388(2) 0.0593(2) 0.0228(9) Uani 1.00 d . . .
  C(9*) C -0.0060(3) 0.1041(2) 0.0330(2) 0.0226(9) Uani 1.00 d . . .
  C(12*) C 0.2619(3) 0.0582(2) 0.0447(2) 0.0262(9) Uani 1.00 d . . .
  O(1*) O -0.3706(2) 0.1478(2) 0.2322(2) 0.0357(9) Uani 1.00 d . . .
  O(10*) O -0.2241(2) 0.2241(2) 0.3464(2) 0.0434(9) Uani 1.00 d . . .
  O(11*) O -0.2636(2) 0.0038(2) 0.2370(2) 0.0410(9) Uani 1.00 d . . .
  C(3*) C -0.3151(3) 0.1617(2) 0.1020(2) 0.0279(10) Uani 1.00 d . . .
  C(11*) C 0.1610(3) 0.0674(2) 0.0198(2) 0.0281(10) Uani 1.00 d . . .
  O(6*) O -0.0972(2) 0.2958(2) 0.1360(2) 0.0429(9) Uani 1.00 d . . .
  O(7*) O 0.0296(3) 0.3413(2) 0.0956(2) 0.062(1) Uani 1.00 d . . .
  C(6*) C -0.1915(3) 0.1478(2) -0.0252(2) 0.0298(10) Uani 1.00 d . . .
  C(8*) C -0.0363(3) 0.1113(2) -0.0521(3) 0.032(1) Uani 1.00 d . . .
  C(13*) C 0.3220(3) 0.0305(3) -0.0175(3) 0.036(1) Uani 1.00 d . . .
  C(2*) C -0.3863(3) 0.1632(3) 0.1564(3) 0.032(1) Uani 1.00 d . . .
  C(14*) C -0.265(1) 0.2646(8) 0.404(1) 0.073(5) Uani 0.50 d P . .
  C(14'*) C -0.2848(8) 0.2860(7) 0.338(1) 0.070(4) Uani 0.50 d P . .
  H(12*) H -0.1638 0.2432 0.3379 0.0360 Uiso 1.00 calc . . .
  C(15*) C -0.3371(5) -0.0484(4) 0.2471(4) 0.066(2) Uani 1.00 d . . .
  H(16*) H -0.2097 -0.0168 0.2212 0.0360 Uiso 1.00 calc . . .
  H(4*) H -0.3423 0.1700 0.0430 0.0360 Uiso 1.00 calc . . .
  H(8*) H 0.1419 0.0563 -0.0421 0.0360 Uiso 1.00 calc . . .
  C(7*) C -0.1291(3) 0.1343(3) -0.0811(2) 0.036(1) Uani 1.00 d . . .
  H(5*) H -0.2556 0.1651 -0.0450 0.0360 Uiso 1.00 calc . . .
  H(7*) H 0.0127 0.1109 -0.0824 0.0360 Uiso 1.00 calc . . .
  H(9*) H 0.2841 0.0167 -0.0697 0.0360 Uiso 1.00 calc . . .
  H(10*) H 0.3540 0.0712 -0.0317 0.0360 Uiso 1.00 calc . . .
  H(11*) H 0.3492 -0.0118 -0.0003 0.0360 Uiso 1.00 calc . . .
  C(1*) C -0.4866(3) 0.1829(3) 0.1196(3) 0.047(1) Uani 1.00 d . . .
  H(13*) H -0.2285 0.2677 0.4536 0.0883 Uiso 0.50 calc P . .
  H(14*) H -0.3284 0.2465 0.4042 0.0883 Uiso 0.50 calc P . .
  H(15*) H -0.2727 0.3202 0.3833 0.0795 Uiso 1.00 calc . . .
  H(13'*) H -0.2720 0.3169 0.2883 0.0795 Uiso 0.50 calc P . .
  H(14'*) H -0.3492 0.2714 0.3266 0.0795 Uiso 0.50 calc P . .
  H(17*) H -0.3509 -0.0936 0.2073 0.0360 Uiso 1.00 calc . . .
  H(18*) H -0.3276 -0.0742 0.3023 0.0360 Uiso 1.00 calc . . .
  H(19*) H -0.4043 -0.0226 0.2158 0.0360 Uiso 1.00 calc . . .
  H(6*) H -0.1487 0.1448 -0.1398 0.0360 Uiso 1.00 calc . . .
  H(1*) H -0.5295 0.1601 0.1387 0.0360 Uiso 1.00 calc . . .
  H(2*) H -0.5159 0.2257 0.1358 0.0360 Uiso 1.00 calc . . .
  H(3*) H -0.5075 0.1877 0.0650 0.0360 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_formula_sum        'C30 H38 N5 O21 Ni2 Tb '
_cod_database_code               4307440