Sterically crowded diphosphinomethane ligands: molecular structures, UV-photoelectron spectroscopy and a convenient general synthesis of tBu2PCH2PtBu2 and related species
Eisenträger, Frank; Göthlich, Alexander; Gruber, Irene; Heiss, Helmut; Kiener, Christoph A.; Krüger, Carl; Ulrich Notheis, J.; Rominger, Frank; Scherhag, Gunter; Schultz, Madeleine; Straub, Bernd F.; Volland, Martin A. O.; Hofmann, Peter; New Journal of Chemistry 27 (2003) 540–550; doi:10.1039/b210114a

data_7050496
_publ_section_title
;
 Sterically crowded diphosphinomethane ligands: molecular structures,
 UV-photoelectron spectroscopy and a convenient general synthesis of
 tBu2PCH2PtBu2 and related species
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              540
_journal_page_last               550
_journal_paper_doi               10.1039/b210114a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C18 H40 Cl6 Fe P2'
_chemical_formula_weight         586.99
_chemical_name_common            dtbpmCl+
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.8570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2861(3)
_cell_length_b                   9.9887(2)
_cell_length_c                   17.3272(3)
_cell_measurement_temperature    200(2)
_cell_volume                     2894.47(9)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1251
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28351
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .07
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.1019
_refine_ls_shift/su_max          0.877
_refine_ls_shift/su_mean         0.141
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+19.1108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2771
_reflns_number_gt                3776
_reflns_number_total             6617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210114a.txt
_cod_data_source_block           mv15_dtbpmCl+_9
_cod_depositor_comments
;
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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7050496