Synthesis and spectroscopic characterization of a new family of Ni(4) spin clusters.
Sieber, Andreas; Boskovic, Colette; Bircher, Roland; Waldmann, Oliver; Ochsenbein, Stefan T.; Chaboussant, Grégory; Güdel, Hans U; Kirchner, Nadeschda; van Slageren, Joris; Wernsdorfer, Wolfgang; Neels, Antonia; Stoeckli-Evans, Helen; Janssen, Stefan; Juranyi, Fanni; Mutka, Hannu; Inorganic chemistry 44 (2005) 4315–4325; doi:10.1021/ic050134j

data_4340432
_publ_section_title
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 Synthesis and spectroscopic characterization of a new family of Ni(4)
 spin clusters.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4315
_journal_page_last               4325
_journal_paper_doi               10.1021/ic050134j
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H52 N4 Ni4 O12'
_chemical_formula_weight         1015.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.582(11)
_cell_angle_beta                 75.087(11)
_cell_angle_gamma                70.346(11)
_cell_formula_units_Z            2
_cell_length_a                   13.1852(13)
_cell_length_b                   13.6138(13)
_cell_length_c                   14.2325(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.15
_cell_volume                     2169.8(4)
_computing_cell_refinement       'CELL, Stoe & Cie Company, Germany'
_computing_data_collection       'EXPOSE, Stoe & Cie Company, Germany'
_computing_data_reduction        'INTEGRATE, Stoe & Cie Company, Germany'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'IPDS, Stoe & Cie Company, Germany'
_diffrn_measurement_method       'phi oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16625
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (PLATON99, Spek, 1990)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         7888
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                5786
_reflns_number_total             7888
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic050134jsi20050127_110149.cif
_cod_data_source_block           compound_1b
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4340432