Phosphino-urea chemistry: preparation and structure of chelate and P–N bond cleavage complexes
Slawin, Alexandra M. Z.; Wainwright, Matthew; Derek Woollins, J.; New Journal of Chemistry 24 (2000) 69–; doi:10.1039/a908153d

data_7051246
_publ_section_title
;
 Phosphino-urea chemistry: preparation and structure of chelate and
 P--N bond cleavage complexes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              69
_journal_paper_doi               10.1039/a908153d
_journal_volume                  24
_journal_year                    2000
_chemical_formula_analytical     'C56 H58 Cl4 N4 O5 P4 Pd2'
_chemical_formula_moiety         'C56 H58 Cl4 N4 O5 P4 Pd2'
_chemical_formula_structural     'C56 H58 Cl4 N4 O5 P4 Pd2'
_chemical_formula_sum            'C56 H58 Cl4 N4 O5 P4 Pd2'
_chemical_formula_weight         1345.54
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.1840(10)
_cell_angle_beta                 71.8340(10)
_cell_angle_gamma                72.8060(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6946(3)
_cell_length_b                   15.4866(4)
_cell_length_c                   18.5407(3)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      337
_cell_measurement_theta_min      23
_cell_volume                     3007.91(12)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14316
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.773652
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          .06
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .2
_refine_diff_density_max         2.305
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0007(2)
_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   1.022
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8512
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.221
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.8900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1503
_refine_ls_wR_factor_obs         0.1130
_reflns_number_observed          6340
_reflns_number_total             8562
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908153d.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

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^)+(0.0699P)^2^+2.8900P] 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^)+(0.0699P)^2^+2.8900P] 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      P-1
_cod_database_code               7051246