Syntheses, structural studies, photoelectron spectra and density functional theory calculations of the “pseudo” tetraphospha-metallocenes [M(η-P2C3But3)2], (M = Ni, Pd, Pt)
Cloke, F. Geoffrey N.; Green, Jennifer C.; Hitchcock, Peter B.; Nixon, John F.; Suter, James L.; Wilson, D. James; Dalton Transactions  (2009) 1164–1171; doi:10.1039/b815255a

data_7000507
_publ_section_title
;
 Syntheses, structural studies, photoelectron spectra and density
 functional theory calculations of the &#x201C;pseudo&#x201D;
 tetraphospha-metallocenes [M(\h-P2C3But3)2], (M = Ni, Pd, Pt)
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1164
_journal_page_last               1171
_journal_paper_doi               10.1039/b815255a
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H54 P4 Pt'
_chemical_formula_sum            'C30 H54 P4 Pt'
_chemical_formula_weight         733.7
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-08-10T16:24:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.988(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4887(4)
_cell_length_b                   15.3795(4)
_cell_length_c                   15.2504(4)
_cell_measurement_reflns_used    11489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     3372.99(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22145
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    4.366
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.182
_refine_diff_density_min         -3.376
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         7982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+18.5204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                5553
_reflns_number_total             7982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815255a.txt
_cod_data_source_block           aug499
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7000507