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_7114699
_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            'C97 H150 N4 Ni14.08 O31 Pt9.92'
_chemical_formula_weight         4630.48
_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                 98.4040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.7155(9)
_cell_length_b                   15.2758(5)
_cell_length_c                   31.9982(11)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.33
_cell_measurement_theta_min      1.25
_cell_volume                     12918.3(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      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1347
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            111119
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    12.755
_exptl_absorpt_correction_T_max  0.246
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             8705
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.158
_refine_diff_density_min         -1.788
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         21957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                10701
_reflns_number_total             21957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103610f.txt
_cod_data_source_block           mon
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               7114699