Combining Azide, Carboxylate, and 2-Pyridyloximate Ligands in Transition-Metal Chemistry: Ferromagnetic NiII5 Clusters with a Bowtie Skeleton
Constantina Papatriantafyllopoulou; Theocharis C. Stamatatos; Wolfgang Wernsdorfer; Simon J. Teat; Anastasios J. Tasiopoulos; Albert Escuer; Spyros P. Perlepes; Inorganic Chemistry 49 (2010) 10486–10496; doi:10.1021/ic1014829

data_4317032
_publ_section_title
;
 Combining Azide, Carboxylate, and 2-Pyridyloximate Ligands in
 Transition-Metal Chemistry: Ferromagnetic NiII5 Clusters with a Bowtie
 Skeleton
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10486
_journal_page_last               10496
_journal_paper_doi               10.1021/ic1014829
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C56 H58.5 N20 Ni5 O12.25'
_chemical_formula_weight         1501.28
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.628(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4167(13)
_cell_length_b                   24.334(2)
_cell_length_c                   19.8508(17)
_cell_measurement_reflns_used    7275
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      33.70
_cell_measurement_theta_min      2.76
_cell_volume                     6930.4(10)
_computing_cell_refinement       'Bruker SAINT v7.23a'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT v7.23a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Platinum 200 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38752
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         33.77
_diffrn_reflns_theta_min         2.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS Madison WI USA'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3090
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10649
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.774
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+4.7220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                8557
_reflns_number_total             10649
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1014829_si_003_2.cif
_cod_data_source_block           ni29
_cod_original_formula_sum        'C56 H58.50 N20 Ni5 O12.25'
_cod_database_code               4317032