A high-nuclearity Ni‒Sb carbonyl cluster displaying unprecedented metal stereochemistries: synthesis and X-ray structure of [NEt4]6[Ni31Sb4(CO)40]·2 Me2CO
Femoni, Cristina; Iapalucci, M. Carmela; Longoni, Giuliano; Svensson, Per H.; Chemical Communications  (2000) 655–; doi:10.1039/b000783h

data_7110871
_publ_contact_author
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Prof. Giuliano Longoni
Viale Risorgimento 4, I-40136 Bologna, Italy
 
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_publ_section_title
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 A high-nuclearity Ni--Sb carbonyl cluster displaying unprecedented metal
 stereochemistries: synthesis and X-ray structure of
 [NEt4]6[Ni31Sb4(CO)40]&#x00B7;2 Me2CO
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_journal_issue                   8
_journal_name_full               'Chemical Communications'
_journal_page_first              655
_journal_paper_doi               10.1039/b000783h
_journal_year                    2000
_chemical_formula_sum            'C94 H132 N6 Ni31 O42 Sb4'
_chemical_formula_weight         4325.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.7070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.9876(6)
_cell_length_b                   14.6084(4)
_cell_length_c                   44.1418(11)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.24
_cell_measurement_theta_min      1.47
_cell_volume                     13505.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            94623
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    5.059
_exptl_absorpt_correction_T_max  0.573
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             8584
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1449
_refine_ls_number_reflns         23779
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                12946
_reflns_number_total             23779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000783hsup1.cif
_cod_data_source_block           '[NEt4]6[Ni31Sb4(CO)40].2Me2CO'
_cod_depositor_comments
;
The following automatic conversions were performed:
'__cell_measurement_theta_max' tag replaced with
'_cell_measurement_theta_max'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110871