Synthesis and characterisation of the first E-unidentate [Ph2P(O)NP(E)Ph2]− metal complexes [Au{Ph2P(O)NP(E)Ph2-E }{Ph2P(O)NHPPh2}] and [Pd{Ph2P(O)NP(E)Ph2-E }2(H2NCH2CH2NH2)] (E = S or Se)
Slawin, Alexandra M. Z.; Smith, Martin B.; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (1998) 1537–; doi:10.1039/a801856a

data_7027842
_publ_section_title
;
 Synthesis and characterisation of the first E-unidentate
 [Ph2P(O)NP(E)Ph2]&#x2212; metal complexes
 [Au{Ph2P(O)NP(E)Ph2-E&#x200A;}{Ph2P(O)NHPPh2}] and
 [Pd{Ph2P(O)NP(E)Ph2-E&#x200A;}2(H2NCH2CH2NH2)] (E&#x2005;=&#x2005;S or
 Se)
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1537
_journal_paper_doi               10.1039/a801856a
_journal_year                    1998
_chemical_formula_sum            'C48.5 H44 Au N2 O3 P4 S'
_chemical_formula_weight         1055.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.3439(10)
_cell_length_b                   13.2267(3)
_cell_length_c                   18.4912(5)
_cell_measurement_temperature    293(2)
_cell_volume                     9619.5(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.1423
_diffrn_reflns_av_sigmaI/netI    0.4592
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20783
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    3.276
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       prism
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          .05
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00115(6)
_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_all   0.403
_refine_ls_goodness_of_fit_obs   0.755
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      8.987
_refine_ls_restrained_S_obs      0.755
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         0.454
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         2.5373
_refine_ls_wR_factor_obs         0.1074
_reflns_number_observed          1974
_reflns_number_total             6926
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a801856sup1.cif
_cod_data_source_block           3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C48.50 H44 Au N2 O3 P4 S'
_cod_database_code               7027842