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_4307431
_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 N5 Nd Ni2 O22'
_chemical_formula_weight         1098.33
_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                92.480(3)
_cell_angle_beta                 104.616(3)
_cell_angle_gamma                91.396(4)
_cell_formula_units_Z            1
_cell_length_a                   7.8223(6)
_cell_length_b                   9.3897(8)
_cell_length_c                   14.454(1)
_cell_measurement_reflns_used    5671
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.5
_cell_volume                     1025.63(14)
_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 0.9846
_diffrn_measured_fraction_theta_max 0.9846
_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  0.038
_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            9508
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.41
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4592
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.07800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                4301
_reflns_number_total             4593
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_04.cif
_cod_data_source_block           4_Ni2Nd_A_[Ni2Nd(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 -0.1016(3) -0.0691(2) -0.1781(1) 0.0221(5) Uani 1.00 d . . .
  O(3*) O 0.1761(3) -0.1779(2) 0.1085(1) 0.0216(5) Uani 1.00 d . . .
  O(5*) O -0.2358(3) -0.1979(2) -0.0156(2) 0.0373(7) Uani 1.00 d . . .
  O(6*) O -0.2744(3) -0.0098(2) 0.0648(2) 0.0357(6) Uani 1.00 d . . .
  N(1*) N 0.0792(3) -0.2575(2) -0.0718(2) 0.0184(5) Uani 1.00 d . . .
  O(4*) O 0.3890(3) -0.2497(2) 0.2973(2) 0.0380(6) Uani 1.00 d . . .
  Ni(*) Ni -0.24961(5) 0.08749(4) -0.24151(3) 0.02237(10) Uani 1.00 d . . .
  O(9*) O -0.1212(9) 0.4357(9) 0.4369(5) 0.068(2) Uani 0.50 d P . .
  O(13*) O 0.119(2) 0.649(1) 0.4254(7) 0.083(4) Uani 0.50 d P . .
  H(20*) H 0.1083 0.5516 0.4399 0.0971 Uiso 0.50 calc P . .
  O(8*) O 0.038(1) 0.4445(8) 0.5796(5) 0.078(3) Uani 0.50 d P . .
  C(16*) C 0.214(2) 0.729(2) 0.5126(10) 0.076(4) Uani 0.50 d P . .
  O(8*) O 1.038(1) 0.4445(8) 0.5796(5) 0.078(3) Uani 0.50 d P . .
  O(10*) O 0.818(2) 0.302(2) 0.537(1) 0.129(7) Uani 0.50 d P . .
  N(3*) N 0.9081(9) 0.3944(9) 0.5197(5) 0.050(2) Uani 0.50 d P . .
  C(4*) C -0.0773(4) -0.1843(3) -0.2257(2) 0.0217(6) Uani 1.00 d . . .
  C(10*) C 0.2203(4) -0.3049(3) 0.0900(2) 0.0200(6) Uani 1.00 d . . .
  N(2*) N -0.3213(3) -0.1369(3) 0.0369(2) 0.0278(6) Uani 1.00 d . . .
  C(5*) C 0.0335(4) -0.2906(3) -0.1666(2) 0.0214(6) Uani 1.00 d . . .
  C(9*) C 0.1743(4) -0.3498(3) -0.0139(2) 0.0204(6) Uani 1.00 d . . .
  C(12*) C 0.3868(4) -0.3686(3) 0.2543(2) 0.0298(8) Uani 1.00 d . . .
  O(1*) O -0.3212(3) -0.0154(3) -0.3686(2) 0.0343(6) Uani 1.00 d . . .
  O(11*) O -0.4706(3) 0.0019(3) -0.2025(2) 0.0458(7) Uani 1.00 d . . .
  O(12*) O -0.0401(4) 0.1910(3) -0.2810(2) 0.0378(7) Uani 1.00 d . . .
  N(3*) N -0.0919(9) 0.3944(9) 0.5197(5) 0.050(2) Uani 0.50 d P . .
  O(13') O -0.119(2) 0.351(1) 0.5746(7) 0.083(4) Uani 0.50 d P . .
  H(20') H -0.1083 0.4484 0.5601 0.0971 Uiso 0.50 calc P . .
  H(21*) H 0.2733 0.8131 0.5000 0.0973 Uiso 0.50 calc P . .
  H(22*) H 0.3022 0.6724 0.5535 0.0973 Uiso 0.50 calc P . .
  H(23*) H 0.1339 0.7578 0.5508 0.0973 Uiso 0.50 calc P . .
  O(9') O 1.1212(9) 0.5643(9) 0.5631(5) 0.068(2) Uani 0.50 d P . .
  O(9*) O 0.8788(9) 0.4357(9) 0.4369(5) 0.068(2) Uani 0.50 d P . .
  C(3*) C -0.1472(5) -0.2159(4) -0.3220(2) 0.0322(8) Uani 1.00 d . . .
  C(11*) C 0.3068(4) -0.3987(3) 0.1558(2) 0.0263(7) Uani 1.00 d . . .
  O(7*) O -0.4400(3) -0.1994(3) 0.0614(2) 0.0454(8) Uani 1.00 d . . .
  C(6*) C 0.0869(5) -0.4148(3) -0.2059(2) 0.0325(8) Uani 1.00 d . . .
  C(8*) C 0.2331(5) -0.4765(3) -0.0489(2) 0.0309(8) Uani 1.00 d . . .
  C(13*) C 0.4796(6) -0.4859(4) 0.3126(3) 0.0456(10) Uani 1.00 d . . .
  C(2*) C -0.2628(4) -0.1313(4) -0.3887(2) 0.0335(8) Uani 1.00 d . . .
  C(14*) C -0.5438(5) -0.1392(4) -0.2234(4) 0.052(1) Uani 1.00 d . . .
  H(12*) H -0.5129 0.0463 -0.1619 0.0302 Uiso 1.00 calc . . .
  C(15*) C 0.1094(6) 0.1247(5) -0.2980(3) 0.052(1) Uani 1.00 d . . .
  H(16*) H -0.0665 0.2435 -0.3320 0.0302 Uiso 1.00 calc . . .
  O(10*) O -0.182(2) 0.302(2) 0.537(1) 0.129(7) Uani 0.50 d P . .
  C(16') C -0.214(2) 0.271(2) 0.4874(10) 0.076(4) Uani 0.50 d P . .
  N(3') N 1.0919(9) 0.6056(9) 0.4803(5) 0.050(2) Uani 0.50 d P . .
  O(8') O 0.962(1) 0.5555(8) 0.4204(5) 0.078(3) Uani 0.50 d P . .
  H(4*) H -0.1145 -0.3036 -0.3468 0.0388 Uiso 1.00 calc . . .
  H(8*) H 0.3133 -0.4940 0.1322 0.0317 Uiso 1.00 calc . . .
  C(7*) C 0.1881(5) -0.5076(3) -0.1457(2) 0.0373(9) Uani 1.00 d . . .
  H(5*) H 0.0540 -0.4348 -0.2731 0.0393 Uiso 1.00 calc . . .
  H(7*) H 0.3024 -0.5395 -0.0062 0.0371 Uiso 1.00 calc . . .
  H(9*) H 0.4687 -0.5710 0.2732 0.0545 Uiso 1.00 calc . . .
  H(10*) H 0.4269 -0.5016 0.3640 0.0545 Uiso 1.00 calc . . .
  H(11*) H 0.6007 -0.4592 0.3374 0.0545 Uiso 1.00 calc . . .
  C(1*) C -0.3241(8) -0.1906(6) -0.4895(3) 0.069(1) Uani 1.00 d . . .
  H(13*) H -0.4567 -0.2050 -0.1982 0.0625 Uiso 1.00 calc . . .
  H(14*) H -0.6411 -0.1501 -0.1959 0.0625 Uiso 1.00 calc . . .
  H(15*) H -0.5835 -0.1557 -0.2911 0.0625 Uiso 1.00 calc . . .
  H(17*) H 0.0736 0.0543 -0.3489 0.0638 Uiso 1.00 calc . . .
  H(18*) H 0.1863 0.1937 -0.3140 0.0638 Uiso 1.00 calc . . .
  H(19*) H 0.1707 0.0799 -0.2416 0.0638 Uiso 1.00 calc . . .
  H(21') H -0.2733 0.1869 0.5000 0.0973 Uiso 0.50 calc P . .
  H(22') H -0.3022 0.3276 0.4465 0.0973 Uiso 0.50 calc P . .
  H(23') H -0.1339 0.2422 0.4492 0.0973 Uiso 0.50 calc P . .
  O(10') O 1.182(2) 0.698(2) 0.463(1) 0.129(7) Uani 0.50 d P . .
  O(13*) O 1.119(2) 0.649(1) 0.4254(7) 0.083(4) Uani 0.50 d P . .
  C(16*) C 1.214(2) 0.729(2) 0.5126(10) 0.076(4) Uani 0.50 d P . .
  H(20*) H 1.1083 0.5516 0.4399 0.0971 Uiso 0.50 calc P . .
  H(6*) H 0.2259 -0.5928 -0.1711 0.0447 Uiso 1.00 calc . . .
  H(1*) H -0.4485 -0.2032 -0.5058 0.0810 Uiso 1.00 calc . . .
  H(2*) H -0.2902 -0.1248 -0.5307 0.0810 Uiso 1.00 calc . . .
  H(3*) H -0.2707 -0.2786 -0.4951 0.0810 Uiso 1.00 calc . . .
  H(21*) H 1.2733 0.8131 0.5000 0.0973 Uiso 0.50 calc P . .
  H(22*) H 1.3022 0.6724 0.5535 0.0973 Uiso 0.50 calc P . .
  H(23*) H 1.1339 0.7578 0.5508 0.0973 Uiso 0.50 calc P . .

  Andrius Merkys
  2013-11-08
;
_cod_original_cell_volume        1025.6(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H42 N5 Nd O22 Ni2 '
_cod_database_code               4307431