Orthopalladation of iminophosphoranes: synthesis, structure and study of stability
Bielsa, Raquel; Navarro, Rafael; Soler, Tatiana; Urriolabeitia, Esteban P.; Dalton Transactions  (2008) 1203–1214; doi:10.1039/b714485g

data_7003215
_publ_section_title
;
 Orthopalladation of iminophosphoranes: synthesis, structure and study
 of stability
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1203
_journal_page_last               1214
_journal_paper_doi               10.1039/b714485g
_journal_year                    2008
_chemical_formula_moiety         'C42 H38 Cl2 N2 O4 P2 Pd2, 2(C H Cl3)'
_chemical_formula_sum            'C44 H40 Cl8 N2 O4 P2 Pd2'
_chemical_formula_weight         1219.12
_chemical_name_systematic
;
?
;
_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                 99.8661(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9958(2)
_cell_length_b                   13.5663(3)
_cell_length_c                   14.8552(2)
_cell_measurement_reflns_used    15006
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      33.57
_cell_measurement_theta_min      4.25
_cell_volume                     2381.76(7)
_computing_cell_refinement
;
CrysAlis RED (Oxford, 2005)
;
_computing_data_collection
;
CrysAlis CCD (Oxford, 2005)
;
_computing_data_reduction
;
CrysAlis RED (Oxford, 2005)
;
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29116
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.8653
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5463
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.316
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+6.8538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                4625
_reflns_number_total             5463
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b714485g.txt
_cod_data_source_block           d123psm
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7003215