Macropolyhedral boron-containing cluster chemistry. Mixed and multiple cluster fusion in platinaborane chemistry and the structure of [(PMe2Ph)2PtB16H17PtB10H11(PMe2Ph)] as determined by synchrotron X-ray diffraction analysis
Bould, Jonathan; Clegg, William; Kennedy, John D.; Teat, Simon J.; Journal of the Chemical Society, Dalton Transactions  (1998) 2777–; doi:10.1039/a803817a

data_7027855
_publ_section_title
;
 Macropolyhedral boron-containing cluster chemistry. Mixed and multiple
 cluster fusion in platinaborane chemistry and the structure of
 [(PMe2Ph)2PtB16H17PtB10H11(PMe2Ph)] as determined by synchrotron X-ray
 diffraction analysis
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2777
_journal_paper_doi               10.1039/a803817a
_journal_year                    1998
_chemical_formula_sum            'C33 H74 B26 P3 Pt2'
_chemical_formula_weight         1235.07
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.452(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7903(4)
_cell_length_b                   13.0595(3)
_cell_length_c                   28.3431(7)
_cell_measurement_reflns_used    21298
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      1.39
_cell_volume                     5474.4(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6874
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            31509
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.219
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.754
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00011(3)
_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   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         11734
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0374P)^2^+13.0171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                9491
_reflns_number_total             11734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            A803817sup1.cif
_cod_data_source_block           jdk1
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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               7027855