Highly Selective Hydrocyanation of Butadiene toward 3-Pentenenitrile
Laura Bini; Christian Müller; Jos Wilting; Lars von Chrzanowski; Anthony L. Spek; Dieter Vogt; Journal of the American Chemical Society 129 (2007) 12622–12623; doi:10.1021/ja074922e

data_4110050
_publ_contact_author_address
;
Bijvoet Center for Biomolecular Research
Crystal and Structural Chemistry
Utrecht University
Padualaan 8
3584 CH Utrecht
The Netherlands
;
_publ_contact_author_email       l.vonchrzanowski@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Lars S. von Chrzanowski'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Highly Selective Hydrocyanation of Butadiene toward 3-Pentenenitrile
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12622
_journal_page_last               12623
_journal_paper_doi               10.1021/ja074922e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C44 H32 Cl2 P2 Pt, 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H36 Cl6 P2 Pt'
_chemical_formula_weight         1058.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.14097(18)
_cell_length_b                   16.8563(3)
_cell_length_c                   15.2270(4)
_cell_measurement_reflns_used    15463
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.75
_cell_volume                     4142.92(14)
_computing_cell_refinement       PEAKREF
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 Altomare et al. (1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18011
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  0.5069
_exptl_absorpt_correction_T_min  0.2788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         1.128
_refine_diff_density_min         -4.118
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 1724 Friedel pairs'
_refine_ls_abs_structure_Flack   0.048(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3802
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+13.4692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                3734
_reflns_number_total             3802
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja074922erom20070704_091428.cif
_cod_data_source_block           s3818a
_cod_original_cell_volume        4142.93(14)
_cod_database_code               4110050