Single-molecule magnet behavior in three cyano-bridged heterometallic Fe(III)-Ni(II) clusters.
Zhuang, Peng-Fei; Zhang, Yan-Juan; Zheng, Hui; Jiao, Cheng-Qi; Zhao, Liang; Wang, Jun-Li; He, Cheng; Duan, Chun-Ying; Liu, Tao; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3393–3398; doi:10.1039/c4dt03365e

data_7033564
_publ_section_title
;
 Single-molecule magnet behavior in three cyano-bridged heterometallic
 Fe(III)-Ni(II) clusters.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3393
_journal_page_last               3398
_journal_paper_doi               10.1039/c4dt03365e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C29 H32 B Fe N15 Ni0.5, C29 H29 B Fe N15 Ni0.5, C O'
_chemical_formula_sum            'C59 H61 B2 Fe2 N30 Ni O'
_chemical_formula_weight         1398.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2014-12-31 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                107.848(2)
_cell_angle_beta                 96.552(2)
_cell_angle_gamma                105.634(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9157(5)
_cell_length_b                   16.0385(5)
_cell_length_c                   21.0439(7)
_cell_measurement_reflns_used    6339
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.22
_cell_volume                     3600.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24942
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.817
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         12673
_refine_ls_number_restraints     1764
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8996
_reflns_number_total             12673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03365e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7033564--7033566.cif.'
_cod_database_code               7033564
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C48-C49 = C49-C50 = C20-C21 = C27-C28 = C19-C20 = C50-C51
 1.45 with sigma of 0.01
 C21-C22 = C19-C20' = C20'-C21' = C21'-C22'
 1.45 with sigma of 0.01
 C26-C27 = C27-C28 = C28-C29 = C26-C27' = C27'-C28' = C28'-C29'
 1.45 with sigma of 0.01
 C48-C49' = C49'-C50' = C50'-C51'
 1.45 with sigma of 0.01
 C55-C56 = C56-C57 = C57-C58 = C55-C56' = C56'-C57' = C57'-C58'
 1.45 with sigma of 0.01
3. Rigid bond restraints
 C55, C56, C20, C21, C22
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9
\\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim N15 \\sim N16 \\sim N18
\\sim N19 \\sim N20 \\sim N21 \\sim N22 \\sim N23 \\sim N24 \\sim N25 \\sim N26
\\sim N27 \\sim N28 \\sim N29 \\sim N30 \\sim N17 \\sim N17': within 3.8A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C20' \\sim C21' \\sim
C22' \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29
\\sim C27' \\sim C28' \\sim C29' \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C49'
\\sim C50' \\sim C51' \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C56' \\sim C57' \\sim C58' \\sim C30 \\sim C31 \\sim C32
\\sim C30' \\sim C31' \\sim C32' \\sim C59: within 4A with sigma of 0.04 and
sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(C56') \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C49) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C20(0.62015) H20A(0.62015) H20B(0.62015) C21(0.62015)
 H21A(0.62015) H21B(0.62015) C22(0.62015) H22A(0.62015) H22B(0.62015)
 H22C(0.62015) C20'(0.37985) H20C(0.37985) H20D(0.37985) C21'(0.37985)
 H21C(0.37985) H21D(0.37985) C22'(0.37985) H22D(0.37985) H22E(0.37985)
 H22F(0.37985) C27(0.62015) H27A(0.62015) H27B(0.62015) C28(0.62015)
 H28A(0.62015) H28B(0.62015) C29(0.62015) H29A(0.62015) H29B(0.62015)
 H29C(0.62015) C27'(0.37985) H27C(0.37985) H27D(0.37985) C28'(0.37985)
 H28C(0.37985) H28D(0.37985) C29'(0.37985) H29D(0.37985) H29E(0.37985)
 H29F(0.37985) C49(0.62015) H49A(0.62015) H49B(0.62015) C50(0.62015)
 H50A(0.62015) H50B(0.62015) C51(0.62015) H51A(0.62015) H51B(0.62015)
 H51C(0.62015) C49'(0.37985) H49C(0.37985) H49D(0.37985) C50'(0.37985)
 H50C(0.37985) H50D(0.37985) C51'(0.37985) H51D(0.37985) H51E(0.37985)
 H51F(0.37985) C56(0.62015) H56A(0.62015) H56B(0.62015) C57(0.62015)
 H57A(0.62015) H57B(0.62015) C58(0.62015) H58A(0.62015) H58B(0.62015)
 H58C(0.62015) C56'(0.37985) H56C(0.37985) H56D(0.37985) C57'(0.37985)
 H57C(0.37985) H57D(0.37985) C58'(0.37985) H58D(0.37985) H58E(0.37985)
 H58F(0.37985) N17(0.62015) C30(0.62015) C31(0.62015) C32(0.62015)
 N17'(0.37985) C30'(0.37985) C31'(0.37985) C32'(0.37985)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C20'(H20C,H20D), C21'(H21C,H21D), C27(H27A,
 H27B), C28(H28A,H28B), C27'(H27C,H27D), C28'(H28C,H28D), C49(H49A,H49B),
 C50(H50A,H50B), C49'(H49C,H49D), C50'(H50C,H50D), C56(H56A,H56B), C57(H57A,
 H57B), C56'(H56C,H56D), C57'(H57C,H57D)
6.b Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C22'(H22D,H22E,H22F), C29(H29A,H29B,H29C), C29'(H29D,
 H29E,H29F), C51(H51A,H51B,H51C), C51'(H51D,H51E,H51F), C58(H58A,H58B,H58C),
 C58'(H58D,H58E,H58F)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
  C25(H25), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C45(H45), C46(H46), C47(H47), C52(H52), C53(H53),
  C54(H54)
;
_shelx_res_checksum              83023
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'