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_4340283
_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
;
 C57 H56 Br6 N8 Ni4 O11, 1.5(C H4 O),C2 H3 N, H2 O
;
_chemical_formula_sum            'C60.5 H67 Br6 N9 Ni4 O13.5'
_chemical_formula_weight         1850.53
_chemical_name_systematic
;
 ?
;
_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                77.946(2)
_cell_angle_beta                 84.651(2)
_cell_angle_gamma                68.156(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7152(11)
_cell_length_b                   12.7462(11)
_cell_length_c                   23.427(2)
_cell_measurement_reflns_used    2282
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.24
_cell_volume                     3446.0(5)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Saint'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58267
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    4.622
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.745926
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1846
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         14090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0374P)^2^+19.2973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                9517
_reflns_number_total             14090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051194ssi20050718_060701.cif
_cod_data_source_block           3&#x00B7;1.5MeOH&#x00B7;MeCN&#x00B7;H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_formula_sum        'C60.50 H67 Br6 N9 Ni4 O13.50'
_cod_database_code               4340283