Crystal structures of diiodidobis[(1<i>S</i>,5<i>S</i>)-4-mesityl-1,2,8,8-tetramethyl-2,4-diazabicyclo[3.2.1]octan-3-ylidene-κ<i>C</i>^3^]palladium(IV) and dichlorido[(1<i>S</i>,5<i>S</i>)-4-mesityl-1,2,8,8-tetramethyl-2,4-diazabicyclo[3.2.1]octan-3-ylidene-κ<i>C</i>^3^](triphenylphosphane-κ<i>P</i>)palladium(IV)
Rais, Eduard; Flörke, Ulrich; Wilhelm, René; Acta Crystallographica Section E 71 (2015) 919–922; doi:10.1107/S2056989015013055

data_2240917
_publ_section_title
;
 Crystal structures of
 diiodidobis[(1<i>S</i>,5<i>S</i>)-4-mesityl-1,2,8,8-tetramethyl-2,4-diazabicyclo[3.2.1]octan-3-ylidene-\k<i>C</i>^3^]palladium(IV)
 and
 dichlorido[(1<i>S</i>,5<i>S</i>)-4-mesityl-1,2,8,8-tetramethyl-2,4-diazabicyclo[3.2.1]octan-3-ylidene-\k<i>C</i>^3^](triphenylphosphane-\k<i>P</i>)palladium(IV)
;
_journal_coeditor_code           WM5179
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              919
_journal_page_last               922
_journal_paper_doi               10.1107/S2056989015013055
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Pd (C19 H28 N2)2 I2 ]'
_chemical_formula_moiety         'C38 H56 I2 N4 Pd'
_chemical_formula_sum            'C38 H56 I2 N4 Pd'
_chemical_formula_weight         929.07
_chemical_name_systematic
Diiodidobis[(1<i>S</i>,5<i>S</i>)-4-mesityl-1,2,8,8-tetramethyl-2,4-diazabicyclo[3.2.1]octan-3-ylidene-\k<i>C</i>^3^]palladium(IV)
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_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                   12.2480(13)
_cell_length_b                   13.3786(14)
_cell_length_c                   23.465(2)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.224
_cell_volume                     3845.0(7)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and local programs
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36757
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.119
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2002)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.326
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3583 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.012(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         9177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                8551
_reflns_number_total             9177
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5179sup1.cif
_cod_data_source_block           I
_cod_database_code               2240917
_cod_database_fobs_code 2240917