N-Phosphino-amidines and -guanidines: synthesis, structure and P,N-chelate chemistry
Baiget, Lise; Batsanov, Andrei S.; Dyer, Philip W.; Fox, Mark A.; Hanton, Martin J.; Howard, Judith A. K.; Lane, Philip K.; Solomon, Sophia A.; Dalton Transactions  (2008) 1043–1054; doi:10.1039/b715736c

data_7003357
_publ_section_title
;
 N-Phosphino-amidines and -guanidines: synthesis, structure and
 P,N-chelate chemistry
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1043
_journal_page_last               1054
_journal_paper_doi               10.1039/b715736c
_journal_year                    2008
_chemical_formula_moiety         'C26 H35 Cl2 N2 P Pd,C D Cl3'
_chemical_formula_sum            'C27 H35 Cl5 D N2 P Pd'
_chemical_formula_weight         704.20
_chemical_name_systematic
;N,N'-Dicyclohexyl-N-diphenylphosphino-acetamidine
palladium dichloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.13(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0573(5)
_cell_length_b                   22.9880(17)
_cell_length_c                   16.8757(10)
_cell_measurement_reflns_used    7104
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.61
_cell_measurement_theta_min      2.44
_cell_volume                     3094.3(4)
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL version 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area detector'
_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  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53693
_diffrn_reflns_theta_full        33.50
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.8826
_exptl_absorpt_correction_T_min  0.7482
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP 6.14 (Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapetzoid
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         13064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+2.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                10165
_reflns_number_total             13064
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b715736c.txt
_cod_data_source_block           15
_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      'P 21/n'
_cod_database_code               7003357