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_7027843
_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            'C52 H53 N4 O2.5 P4 Pd Se2'
_chemical_formula_weight         1162.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                97.07(3)
_cell_angle_beta                 94.37(4)
_cell_angle_gamma                67.02(4)
_cell_formula_units_Z            2
_cell_length_a                   15.403(8)
_cell_length_b                   19.198(8)
_cell_length_c                   10.318(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      31.5
_cell_volume                     2786(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
'DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.01838
_diffrn_orient_matrix_UB_12      -0.03595
_diffrn_orient_matrix_UB_13      0.06894
_diffrn_orient_matrix_UB_21      0.02592
_diffrn_orient_matrix_UB_22      -0.04389
_diffrn_orient_matrix_UB_23      -0.06831
_diffrn_orient_matrix_UB_31      0.06299
_diffrn_orient_matrix_UB_32      0.00403
_diffrn_orient_matrix_UB_33      0.01135
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.13746
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8656
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.14
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -58.80
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            yellow/oraprism
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1174.00
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.52
_refine_ls_extinction_coef       0.0000012(1)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.692
_refine_ls_goodness_of_fit_ref   1.692
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     614
_refine_ls_number_reflns         4537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/esd_max         1.4398
_refine_ls_shift/esd_mean        0.0629
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0529
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                4537
_reflns_number_total             8300
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            a801856sup1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 'w = 1/[\s^2^(Fo) +
0.00022|Fo|^2^]' 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) + 0.00022|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C52 H53 N4 O2.50 P4 Pd Se2 '
_cod_database_code               7027843