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_4307429
_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 H41.5 Ce N5 Ni2 O22'
_chemical_formula_weight         1093.71
_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                92.707(2)
_cell_angle_beta                 104.827(2)
_cell_angle_gamma                91.333(1)
_cell_formula_units_Z            1
_cell_length_a                   7.8217(2)
_cell_length_b                   9.4165(3)
_cell_length_c                   14.5053(5)
_cell_measurement_reflns_used    9251
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     1030.94(6)
_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 0.9885
_diffrn_measured_fraction_theta_max 0.9885
_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  0.020
_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            9448
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    2.079
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.60
_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         4650
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.07900(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                4394
_reflns_number_total             4652
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_02.cif
_cod_data_source_block           2_Ni2Ce_A_[Ni2Ce(L)2(NO3)2(MeOH)4]NO3.MeOH
_cod_depositor_comments
;

  The following atoms were removed from CIF file leaving only atoms from
  asymmetric unit:

  O(2*) O -0.1004(2) -0.0688(2) -0.1794(1) 0.0220(4) Uani 1.00 d . . .
  O(3*) O 0.1747(2) -0.1804(2) 0.1084(1) 0.0224(4) Uani 1.00 d . . .
  O(5*) O -0.2418(3) -0.1990(2) -0.0166(2) 0.0359(5) Uani 1.00 d . . .
  O(6*) O -0.2798(3) -0.0108(2) 0.0644(2) 0.0352(5) Uani 1.00 d . . .
  N(1*) N 0.0785(3) -0.2586(2) -0.0728(1) 0.0187(4) Uani 1.00 d . . .
  O(4*) O 0.3867(3) -0.2519(2) 0.2968(1) 0.0363(5) Uani 1.00 d . . .
  Ni(*) Ni -0.24743(4) 0.08910(3) -0.24174(2) 0.02241(8) Uani 1.00 d . . .
  O(10*) O -0.1234(8) 0.4357(7) 0.4376(4) 0.068(2) Uani 0.50 d P . .
  O(13*) O 0.115(1) 0.647(1) 0.4249(6) 0.081(3) Uani 0.50 d P . .
  C(16*) C 0.213(2) 0.729(1) 0.5116(8) 0.073(3) Uani 0.50 d P . .
  O(8*) O 0.038(1) 0.4432(7) 0.5782(4) 0.083(2) Uani 0.50 d P . .
  O(9*) O -0.177(1) 0.301(2) 0.5383(9) 0.132(6) Uani 0.50 d P . .
  N(3*) N -0.0922(8) 0.3952(7) 0.5196(4) 0.049(2) Uani 0.50 d P . .
  C(4*) C -0.0764(3) -0.1839(2) -0.2269(2) 0.0214(5) Uani 1.00 d . . .
  C(10*) C 0.2179(3) -0.3083(2) 0.0894(2) 0.0197(5) Uani 1.00 d . . .
  N(2*) N -0.3253(3) -0.1382(2) 0.0367(2) 0.0280(5) Uani 1.00 d . . .
  C(5*) C 0.0344(3) -0.2906(2) -0.1674(2) 0.0216(5) Uani 1.00 d . . .
  C(9*) C 0.1734(3) -0.3514(2) -0.0146(2) 0.0204(5) Uani 1.00 d . . .
  C(12*) C 0.3836(3) -0.3706(3) 0.2534(2) 0.0294(6) Uani 1.00 d . . .
  O(1*) O -0.3203(3) -0.0144(2) -0.3689(1) 0.0334(5) Uani 1.00 d . . .
  O(11*) O -0.4689(3) 0.0040(2) -0.2032(2) 0.0452(6) Uani 1.00 d . . .
  O(12*) O -0.0363(3) 0.1916(2) -0.2802(1) 0.0376(5) Uani 1.00 d . . .
  H(20*) H 0.1128 0.7092 0.3717 0.0815 Uiso 0.25 calc P . .
  H(21*) H 0.1234 0.8128 0.5227 0.0349 Uiso 0.50 calc P . .
  H(22*) H 0.2322 0.6876 0.5698 0.0349 Uiso 0.50 calc P . .
  H(23*) H 0.3142 0.7930 0.5125 0.0349 Uiso 0.50 calc P . .
  C(3*) C -0.1462(4) -0.2153(3) -0.3232(2) 0.0317(6) Uani 1.00 d . . .
  C(11*) C 0.3042(3) -0.4018(3) 0.1552(2) 0.0261(6) Uani 1.00 d . . .
  O(7*) O -0.4429(3) -0.2013(2) 0.0627(2) 0.0461(6) Uani 1.00 d . . .
  C(6*) C 0.0888(4) -0.4135(3) -0.2074(2) 0.0327(6) Uani 1.00 d . . .
  C(8*) C 0.2329(4) -0.4766(3) -0.0503(2) 0.0306(6) Uani 1.00 d . . .
  C(13*) C 0.4759(5) -0.4875(3) 0.3126(2) 0.0453(8) Uani 1.00 d . . .
  C(2*) C -0.2620(4) -0.1313(3) -0.3891(2) 0.0324(6) Uani 1.00 d . . .
  C(14*) C -0.5421(4) -0.1366(3) -0.2247(3) 0.0483(9) Uani 1.00 d . . .
  H(12*) H -0.5021 0.0388 -0.1450 0.0316 Uiso 1.00 calc . . .
  C(15*) C 0.1113(5) 0.1232(4) -0.2977(3) 0.0500(10) Uani 1.00 d . . .
  H(16*) H -0.1023 0.2414 -0.3165 0.0316 Uiso 1.00 calc . . .
  H(4*) H -0.1122 -0.3034 -0.3478 0.0361 Uiso 1.00 calc . . .
  H(8*) H 0.3196 -0.5016 0.1282 0.0316 Uiso 1.00 calc . . .
  C(7*) C 0.1897(4) -0.5072(3) -0.1473(2) 0.0367(7) Uani 1.00 d . . .
  H(5*) H 0.0724 -0.4276 -0.2710 0.0316 Uiso 1.00 calc . . .
  H(7*) H 0.2822 -0.5406 -0.0149 0.0316 Uiso 1.00 calc . . .
  H(9*) H 0.4155 -0.5763 0.2902 0.0530 Uiso 1.00 calc . . .
  H(10*) H 0.5940 -0.4909 0.3077 0.0530 Uiso 1.00 calc . . .
  H(11*) H 0.4754 -0.4686 0.3777 0.0530 Uiso 1.00 calc . . .
  C(1*) C -0.3262(6) -0.1892(4) -0.4910(2) 0.069(1) Uani 1.00 d . . .
  H(13*) H -0.5129 -0.1772 -0.2802 0.0565 Uiso 0.50 calc P . .
  H(13'*) H -0.4197 -0.2199 -0.2103 0.0316 Uiso 0.50 calc P . .
  H(14*) H -0.6673 -0.1367 -0.2361 0.0565 Uiso 0.50 calc P . .
  H(14'*) H -0.6186 -0.1613 -0.1868 0.0316 Uiso 0.50 calc P . .
  H(15*) H -0.4958 -0.1955 -0.1725 0.0565 Uiso 0.50 calc P . .
  H(15'*) H -0.6158 -0.1346 -0.2941 0.0316 Uiso 0.50 calc P . .
  H(17*) H 0.0743 0.0591 -0.3522 0.0591 Uiso 1.00 calc . . .
  H(18*) H 0.1938 0.1923 -0.3093 0.0591 Uiso 1.00 calc . . .
  H(19*) H 0.1675 0.0724 -0.2439 0.0591 Uiso 1.00 calc . . .
  H(6*) H 0.2140 -0.6095 -0.1732 0.0316 Uiso 1.00 calc . . .
  H(1*) H -0.4376 -0.1549 -0.5198 0.0702 Uiso 1.00 calc . . .
  H(2*) H -0.2428 -0.1609 -0.5261 0.0702 Uiso 1.00 calc . . .
  H(3*) H -0.3322 -0.2911 -0.4931 0.0702 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-07
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H41.50 Ce N5 O22 Ni2 '
_cod_database_code               4307429