New topologies in pentanuclear nickel/oximato clusters: structural and magnetic characterization.
Esteban, Jordi; Font-Bardia, Mercè; Costa, José Sánchez; Teat, Simon J.; Escuer, Albert; Inorganic chemistry 53 (2014) 3194–3203; doi:10.1021/ic500057j

data_4337615
_publ_section_title
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 New topologies in pentanuclear nickel/oximato clusters: structural and
 magnetic characterization.
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_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3194
_journal_page_last               3203
_journal_paper_doi               10.1021/ic500057j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C31 H45 Br3 N9 Ni5 O13), 3(C H4 O), H2 O'
_chemical_formula_sum            'C65 H104 Br6 N18 Ni10 O30'
_chemical_formula_weight         2684.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.210(7)
_cell_length_b                   15.210(7)
_cell_length_c                   40.38(2)
_cell_measurement_reflns_used    4872
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     8090(7)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_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  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27340
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.25
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4050
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00089(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0668P)^2^+10.4331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                4439
_reflns_number_total             5531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500057j_si_001.cif
_cod_data_source_block           joom65a
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/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 
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_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4337615