Two-Dimensional Coordination Polymers Constructed by [NiIILnIII] Nodes and [WIV(bpy)(CN)6]2- Spacers: A Network of [NiIIDyIII] Single Molecule Magnets
Maria-Gabriela Alexandru; Diana Visinescu; Sergiu Shova; Francesc Lloret; Miguel Julve; Marius Andruh; Inorganic Chemistry 52 (2013) 11627–11637; doi:10.1021/ic4019794

data_4336375
_publ_contact_author_name
;
;
_publ_section_title
;
 Two-Dimensional Coordination Polymers Constructed by [NiIILnIII] Nodes
 and [WIV(bpy)(CN)6]2- Spacers: A Network of [NiIIDyIII] Single Molecule
 Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11627
_journal_page_last               11637
_journal_paper_doi               10.1021/ic4019794
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C35 H30 Gd N11 Ni O8 W, 2.5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C40 H41.5 Gd N13.5 Ni O10 W'
_chemical_formula_weight         1271.18
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-02
_audit_creation_method
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  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.966(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4542(7)
_cell_length_b                   22.6068(7)
_cell_length_c                   15.7197(8)
_cell_measurement_reflns_used    6706
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5256
_cell_measurement_theta_min      2.3521
_cell_volume                     4763.7(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
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SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -64.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789    0.0000 -180.0000 62

  2 omega  -22.00   20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000  -30.0000 42

  3 omega  -14.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000  150.0000 26

  4 omega  -18.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5914 -106.0000 -139.0000 68

  5 omega  -38.00   18.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5914  -57.0000  -30.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0447429000
_diffrn_orient_matrix_UB_12      -0.0002864000
_diffrn_orient_matrix_UB_13      0.0086732000
_diffrn_orient_matrix_UB_21      0.0075214000
_diffrn_orient_matrix_UB_22      -0.0304214000
_diffrn_orient_matrix_UB_23      0.0117111000
_diffrn_orient_matrix_UB_31      0.0272585000
_diffrn_orient_matrix_UB_32      0.0076790000
_diffrn_orient_matrix_UB_33      0.0464206000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24284
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       plate
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         9319
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+14.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                7281
_reflns_number_total             9319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019794_si_004.cif
_cod_data_source_block           shi_1302_maan
_cod_original_formula_sum        'C40 H41.50 Gd N13.50 Ni O10 W'
_cod_database_code               4336375
_chemical_oxdiff_formula         'C34 H40 N6 O10 Ni1 Gd1 W1'
_chemical_oxdiff_usercomment     'Ni_Gd_W, violet 0.2x0.2x0.05'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32