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_4307439
_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 Gd N5 O21 Ni2 '
_chemical_formula_sum            'C30 H38 Gd N5 Ni2 O21'
_chemical_formula_weight         1079.30
_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                 99.328(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.103(1)
_cell_length_b                   17.2153(9)
_cell_length_c                   16.3096(8)
_cell_measurement_reflns_used    17004
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.1
_cell_volume                     3907.4(4)
_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 0.9957
_diffrn_measured_fraction_theta_max 0.9957
_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  0.051
_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            17893
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_exptl_absorpt_coefficient_mu    2.726
_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          0.650
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.28
_refine_diff_density_min         -1.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4428
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.00800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                2956
_reflns_number_total             4439
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic0619153si20061007_020931_12.cif
_cod_data_source_block           7-C_Ni2Gd_C_[Ni2Gd(L)2(NO3)3(MeOH)4]
_cod_depositor_comments
;

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

  O(2*) O -0.1730(2) 0.1422(2) 0.2012(2) 0.0237(10) Uani 1.00 d . . .
  O(3*) O 0.1107(3) 0.0883(2) 0.1520(2) 0.025(1) Uani 1.00 d . . .
  O(5*) O 0.0423(3) 0.2418(2) 0.1761(2) 0.030(1) Uani 1.00 d . . .
  O(8*) O -0.0672(3) -0.0082(2) 0.2079(2) 0.028(1) Uani 1.00 d . . .
  N(1*) N -0.0668(3) 0.1184(3) 0.0872(2) 0.021(1) Uani 1.00 d . . .
  O(4*) O 0.3051(3) 0.0742(2) 0.1153(2) 0.030(1) Uani 1.00 d . . .
  Ni(*) Ni -0.24475(5) 0.11395(5) 0.29226(4) 0.0262(2) Uani 1.00 d . . .
  C(4*) C -0.2193(4) 0.1485(3) 0.1250(3) 0.023(1) Uani 1.00 d . . .
  C(10*) C 0.0935(4) 0.0852(3) 0.0699(3) 0.020(1) Uani 1.00 d . . .
  N(2*) N -0.0103(4) 0.2944(3) 0.1349(3) 0.030(1) Uani 1.00 d . . .
  C(5*) C -0.1566(4) 0.1393(3) 0.0605(3) 0.024(1) Uani 1.00 d . . .
  C(9*) C -0.0064(4) 0.1037(3) 0.0339(3) 0.021(1) Uani 1.00 d . . .
  C(12*) C 0.2617(4) 0.0577(3) 0.0452(3) 0.027(1) Uani 1.00 d . . .
  O(1*) O -0.3705(3) 0.1470(2) 0.2319(2) 0.038(1) Uani 1.00 d . . .
  O(10*) O -0.2254(3) 0.2240(3) 0.3462(3) 0.046(1) Uani 1.00 d . . .
  O(11*) O -0.2635(3) 0.0030(3) 0.2377(2) 0.042(1) Uani 1.00 d . . .
  C(3*) C -0.3161(4) 0.1614(3) 0.1033(3) 0.027(1) Uani 1.00 d . . .
  C(11*) C 0.1605(4) 0.0676(3) 0.0206(3) 0.028(1) Uani 1.00 d . . .
  O(6*) O -0.0964(3) 0.2960(2) 0.1349(2) 0.043(1) Uani 1.00 d . . .
  O(7*) O 0.0286(3) 0.3410(3) 0.0940(3) 0.063(2) Uani 1.00 d . . .
  C(6*) C -0.1908(4) 0.1474(3) -0.0264(3) 0.033(2) Uani 1.00 d . . .
  C(8*) C -0.0370(4) 0.1126(4) -0.0533(3) 0.034(2) Uani 1.00 d . . .
  C(13*) C 0.3201(4) 0.0321(4) -0.0187(3) 0.036(2) Uani 1.00 d . . .
  C(2*) C -0.3872(4) 0.1622(4) 0.1560(3) 0.033(2) Uani 1.00 d . . .
  C(14*) C -0.288(1) 0.2873(9) 0.336(1) 0.063(5) Uani 0.50 d P . .
  C(14'*) C -0.267(1) 0.265(1) 0.401(1) 0.065(6) Uani 0.50 d P . .
  H(12*) H -0.1684 0.2593 0.3233 0.0356 Uiso 0.50 calc P . .
  H(12'*) H -0.1643 0.2429 0.3642 0.0356 Uiso 0.50 calc P . .
  C(15*) C -0.3342(6) -0.0505(4) 0.2502(4) 0.071(3) Uani 1.00 d . . .
  H(16*) H -0.2055 -0.0217 0.2315 0.0356 Uiso 1.00 calc . . .
  H(4*) H -0.3377 0.1717 0.0461 0.0332 Uiso 1.00 calc . . .
  H(8*) H 0.1360 0.0612 -0.0370 0.0345 Uiso 1.00 calc . . .
  C(7*) C -0.1303(4) 0.1331(4) -0.0811(3) 0.037(2) Uani 1.00 d . . .
  H(5*) H -0.2562 0.1620 -0.0456 0.0392 Uiso 1.00 calc . . .
  H(7*) H 0.0070 0.1028 -0.0911 0.0395 Uiso 1.00 calc . . .
  H(9*) H 0.2787 0.0204 -0.0693 0.0427 Uiso 1.00 calc . . .
  H(10*) H 0.3644 0.0707 -0.0277 0.0427 Uiso 1.00 calc . . .
  H(11*) H 0.3545 -0.0145 0.0006 0.0427 Uiso 1.00 calc . . .
  C(1*) C -0.4872(4) 0.1813(4) 0.1204(4) 0.050(2) Uani 1.00 d . . .
  H(13*) H -0.2491 0.3194 0.3975 0.0673 Uiso 1.00 calc . . .
  H(14*) H -0.3350 0.2620 0.3866 0.0673 Uiso 1.00 calc . . .
  H(15'*) H -0.3055 0.3016 0.2847 0.0736 Uiso 0.50 calc P . .
  H(15*) H -0.2468 0.2475 0.4551 0.0673 Uiso 0.50 calc P . .
  H(17*) H -0.3971 -0.0265 0.2321 0.0869 Uiso 1.00 calc . . .
  H(18*) H -0.3295 -0.0616 0.3076 0.0869 Uiso 1.00 calc . . .
  H(19*) H -0.3302 -0.0955 0.2193 0.0869 Uiso 1.00 calc . . .
  H(6*) H -0.1518 0.1375 -0.1387 0.0443 Uiso 1.00 calc . . .
  H(1*) H -0.4918 0.1907 0.0625 0.0634 Uiso 1.00 calc . . .
  H(2*) H -0.5070 0.2251 0.1473 0.0634 Uiso 1.00 calc . . .
  H(3*) H -0.5271 0.1378 0.1284 0.0634 Uiso 1.00 calc . . .

  Andrius Merkys
  2013-11-08
;
_cod_original_cell_volume        3907.5(4)
_cod_original_formula_sum        'C30 H38 Gd N5 O21 Ni2 '
_cod_database_code               4307439