First catalytic dihydroamination of a phosphaalkyne. Crystal and molecular structure of trans-[PdCl2{P(PriNH)2CH2But}2]
Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Nixon, John F.; Wilson, D. James; Chemical Communications  (2000) 2387–; doi:10.1039/b007512o

data_7111139
_publ_section_title
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 First catalytic dihydroamination of a phosphaalkyne. Crystal and
 molecular structure of trans-[PdCl2{P(PriNH)2CH2But}2]
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_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2387
_journal_paper_doi               10.1039/b007512o
_journal_year                    2000
_chemical_formula_structural     '[PdCl2{P(NiPr)2(CH2tBu)}2].2(C7H8)'
_chemical_formula_sum            'C36 H66 Cl2 N4 P2 Pd'
_chemical_formula_weight         794.17
_chemical_name_systematic
; 
 ? 
;
_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                90.44(3)
_cell_angle_beta                 103.26(3)
_cell_angle_gamma                95.81(3)
_cell_formula_units_Z            1
_cell_length_a                   7.869(3)
_cell_length_b                   10.919(3)
_cell_length_c                   12.754(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1060.6(7)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5107
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_reflns         5105
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_refine_ls_restrained_S_obs      1.046
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_refine_ls_R_factor_obs          0.0381
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.7742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1041
_refine_ls_wR_factor_obs         0.0991
_reflns_number_observed          4563
_reflns_number_total             5107
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007512osup1.cif
_cod_data_source_block           aug1598
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.7742P] 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^)+(0.0546P)^2^+0.7742P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1060.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111139