Self-assembly of a tetranuclear Ni4 cluster with an S = 4 ground state: the first 3d metal cluster bearing a mu4-eta2:eta2-O,O carbonate ligand.
Fondo, Matilde; Ocampo, Noelia; García-Deibe, Ana M; Vicente, Ramón; Corbella, Montserrat; Bermejo, Manuel R.; Sanmartín, Jesús; Inorganic chemistry 45 (2006) 255–262; doi:10.1021/ic051194s

data_4340281
_publ_section_title
;
 Self-assembly of a tetranuclear Ni4 cluster with an S = 4 ground state:
 the first 3d metal cluster bearing a mu4-eta2:eta2-O,O carbonate ligand.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              255
_journal_page_last               262
_journal_paper_doi               10.1021/ic051194s
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C29 H29 Br3 N4 Ni2 O7, 3(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C35 H42 Br3 N7 Ni2 O9'
_chemical_formula_weight         1061.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.829(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.177(3)
_cell_length_b                   19.091(4)
_cell_length_c                   29.883(7)
_cell_measurement_reflns_used    1746
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.32
_cell_volume                     8578(3)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF 99 (Beurskens, 1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37987
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        'not significant'
_exptl_absorpt_coefficient_mu    3.730
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5252
_exptl_absorpt_correction_type   empyrical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7317
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0636P)^2^+96.7277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                5051
_reflns_number_total             7317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051194ssi20050718_060701.cif
_cod_data_source_block           1&#x00B7;3MeCN&#x00B7;2H2O
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               4340281