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_4307430
_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 H43 N5 Ni2 O22 Pr'
_chemical_formula_weight         1096.01
_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                92.794(2)
_cell_angle_beta                 104.708(4)
_cell_angle_gamma                91.285(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8083(7)
_cell_length_b                   9.3987(6)
_cell_length_c                   14.481(1)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.5
_cell_volume                     1026.02(13)
_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 0.9815
_diffrn_measured_fraction_theta_max 0.9815
_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  0.025
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_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            9293
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4520
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.0022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.08000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                4350
_reflns_number_total             4523
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_03.cif
_cod_data_source_block           3_Ni2Pr_A_[Ni2Pr(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 -0.1009(2) -0.0688(2) -0.1788(1) 0.0210(4) Uani 1.00 d . . .
  O(3*) O 0.1754(2) -0.1791(2) 0.1086(1) 0.0213(4) Uani 1.00 d . . .
  O(5*) O -0.2777(3) -0.0096(2) 0.0642(2) 0.0343(5) Uani 1.00 d . . .
  O(6*) O -0.2384(3) -0.1987(2) -0.0161(2) 0.0357(5) Uani 1.00 d . . .
  N(1*) N 0.0787(3) -0.2581(2) -0.0724(1) 0.0179(4) Uani 1.00 d . . .
  O(4*) O 0.3877(3) -0.2511(2) 0.2968(1) 0.0360(5) Uani 1.00 d . . .
  Ni(*) Ni -0.24855(4) 0.08816(3) -0.24163(2) 0.02114(8) Uani 1.00 d . . .
  O(10*) O 0.9535(9) 0.5565(7) 0.4206(4) 0.075(2) Uani 0.50 d P . .
  O(13*) O 0.883(2) 0.3517(10) 0.5760(6) 0.081(3) Uani 0.50 d P . .
  C(16*) C 0.789(2) 0.271(1) 0.4895(7) 0.072(3) Uani 0.50 d P . .
  O(8*) O 1.1212(8) 0.5648(7) 0.5621(4) 0.068(2) Uani 0.50 d P . .
  H(20*) H 0.9213 0.4469 0.5808 0.0287 Uiso 1.00 calc . . .
  O(9*) O 1.175(1) 0.699(2) 0.4603(9) 0.126(6) Uani 0.50 d P . .
  N(3*) N 1.0904(7) 0.6058(7) 0.4804(4) 0.049(2) Uani 0.50 d P . .
  C(4*) C -0.0771(3) -0.1841(2) -0.2263(2) 0.0196(5) Uani 1.00 d . . .
  C(10*) C 0.2196(3) -0.3068(2) 0.0895(2) 0.0182(5) Uani 1.00 d . . .
  N(2*) N -0.3232(3) -0.1380(2) 0.0370(2) 0.0262(5) Uani 1.00 d . . .
  C(5*) C 0.0340(3) -0.2911(2) -0.1673(2) 0.0202(5) Uani 1.00 d . . .
  C(9*) C 0.1739(3) -0.3511(2) -0.0145(2) 0.0192(5) Uani 1.00 d . . .
  C(12*) C 0.3847(3) -0.3693(3) 0.2536(2) 0.0274(6) Uani 1.00 d . . .
  O(1*) O -0.3209(3) -0.0152(2) -0.3688(1) 0.0323(5) Uani 1.00 d . . .
  O(11*) O -0.4692(3) 0.0025(2) -0.2029(2) 0.0448(6) Uani 1.00 d . . .
  O(12*) O -0.0379(3) 0.1919(2) -0.2805(1) 0.0358(5) Uani 1.00 d . . .
  H(21*) H 0.7072 0.3308 0.4471 0.0939 Uiso 0.50 calc P . .
  H(22*) H 0.8668 0.2323 0.4564 0.0939 Uiso 0.50 calc P . .
  H(23*) H 0.7179 0.1961 0.5058 0.0939 Uiso 0.50 calc P . .
  C(3*) C -0.1462(4) -0.2151(3) -0.3230(2) 0.0306(6) Uani 1.00 d . . .
  C(11*) C 0.3053(3) -0.4003(2) 0.1554(2) 0.0245(6) Uani 1.00 d . . .
  O(7*) O -0.4413(3) -0.2004(2) 0.0621(2) 0.0434(6) Uani 1.00 d . . .
  C(6*) C 0.0885(4) -0.4144(3) -0.2069(2) 0.0312(6) Uani 1.00 d . . .
  C(8*) C 0.2333(4) -0.4771(2) -0.0492(2) 0.0289(6) Uani 1.00 d . . .
  C(13*) C 0.4779(5) -0.4872(3) 0.3120(2) 0.0442(8) Uani 1.00 d . . .
  C(2*) C -0.2623(3) -0.1320(3) -0.3888(2) 0.0314(6) Uani 1.00 d . . .
  C(14*) C -0.5434(4) -0.1374(3) -0.2238(3) 0.0471(9) Uani 1.00 d . . .
  H(12*) H -0.5001 0.0402 -0.1540 0.0287 Uiso 1.00 calc . . .
  C(15*) C 0.1115(5) 0.1232(4) -0.2977(3) 0.0493(9) Uani 1.00 d . . .
  H(16*) H -0.0784 0.2400 -0.3346 0.0287 Uiso 1.00 calc . . .
  H(4*) H -0.1169 -0.3060 -0.3535 0.0287 Uiso 1.00 calc . . .
  H(8*) H 0.3079 -0.4975 0.1272 0.0287 Uiso 1.00 calc . . .
  C(7*) C 0.1891(4) -0.5078(3) -0.1467(2) 0.0355(7) Uani 1.00 d . . .
  H(5*) H 0.0552 -0.4375 -0.2739 0.0287 Uiso 1.00 calc . . .
  H(7*) H 0.3176 -0.5376 -0.0030 0.0287 Uiso 1.00 calc . . .
  H(9*) H 0.4686 -0.5722 0.2726 0.0530 Uiso 1.00 calc . . .
  H(10*) H 0.4233 -0.5036 0.3628 0.0530 Uiso 1.00 calc . . .
  H(11*) H 0.5989 -0.4603 0.3382 0.0530 Uiso 1.00 calc . . .
  C(1*) C -0.3251(6) -0.1910(5) -0.4904(2) 0.070(1) Uani 1.00 d . . .
  H(13*) H -0.4561 -0.1925 -0.2012 0.0287 Uiso 1.00 calc . . .
  H(14*) H -0.6346 -0.1464 -0.1916 0.0287 Uiso 1.00 calc . . .
  H(15*) H -0.5693 -0.1632 -0.2910 0.0287 Uiso 1.00 calc . . .
  H(17*) H 0.0534 0.0674 -0.3564 0.0287 Uiso 1.00 calc . . .
  H(18*) H 0.1718 0.0905 -0.2321 0.0287 Uiso 1.00 calc . . .
  H(19*) H 0.1927 0.2065 -0.3069 0.0287 Uiso 1.00 calc . . .
  H(6*) H 0.2211 -0.5994 -0.1694 0.0287 Uiso 1.00 calc . . .
  H(1*) H -0.2819 -0.2838 -0.4956 0.0846 Uiso 1.00 calc . . .
  H(2*) H -0.4511 -0.1956 -0.5088 0.0846 Uiso 1.00 calc . . .
  H(3*) H -0.2826 -0.1308 -0.5312 0.0846 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_cell_volume        1026.0(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H43 N5 O22 Ni2 Pr '
_cod_database_code               4307430