New high-nuclearity Ni‒Pt carbonyl clusters: synthesis and X-ray structure of the ordered [Ni24Pt14(CO)44]4‒ and the substitutionally Ni/Pt disordered [Ni10(Ni6‒xPtx)Pt8(CO)30]4‒ (x = 1.92) tetraanions
Femoni, Cristina; Carmela Iapalucci, M.; Longoni, Giuliano; Svensson, Per H.; Chemical Communications  (2001) 1776–; doi:10.1039/b103610f

data_7114698
_publ_contact_author             'Prof. Giuliano Longoni'
_publ_section_title
;
 New high-nuclearity Ni--Pt carbonyl clusters: synthesis and X-ray
 structure of the ordered [Ni24Pt14(CO)44]4-- and the substitutionally
 Ni/Pt disordered [Ni10(Ni6--xPtx)Pt8(CO)30]4-- (x = 1.92) tetraanions
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1776
_journal_paper_doi               10.1039/b103610f
_journal_year                    2001
_chemical_formula_sum            'C132 H192 N4 Ni24 O50 Pt14'
_chemical_formula_weight         6775.20
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.4645(8)
_cell_length_b                   18.5814(5)
_cell_length_c                   31.6479(9)
_cell_measurement_reflns_used    3192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.24
_cell_measurement_theta_min      1.46
_cell_volume                     17327.0(8)
_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  0.1468
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            152459
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    13.856
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             12704
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.520
_refine_diff_density_min         -2.447
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         15233
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                7779
_reflns_number_total             15233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103610f.txt
_cod_data_source_block           '[NnBu4]4[Ni24Pt14(CO)44].6THF'
_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 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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_sg_symbol_H-M      Pbca
_cod_database_code               7114698