Effect of chalcogens on CO insertion into the palladium-methyl bond of [(N^N^X)Pd(CH3)](+) (X = O, S, Se) and on CO/ethylene copolymerisation.
Kumar, Kamlesh; Darkwa, James; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20714–20727; doi:10.1039/c5dt03929k

data_7036933
_publ_section_title
;
 Effect of chalcogens on CO insertion into the palladium-methyl bond of
 [(N^N^X)Pd(CH3)](+) (X = O, S, Se) and on CO/ethylene copolymerisation.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20714
_journal_page_last               20727
_journal_paper_doi               10.1039/c5dt03929k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C19 H22 Cl N3 O Pd), C H2 Cl2'
_chemical_formula_sum            'C39 H46 Cl4 N6 O2 Pd2'
_chemical_formula_weight         985.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.11.03 svn.r3071 for OlexSys, GUI svn.r4932)
;
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2015-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                94.752(2)
_cell_angle_beta                 97.174(2)
_cell_angle_gamma                111.388(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9985(7)
_cell_length_b                   9.7348(8)
_cell_length_c                   12.7904(10)
_cell_measurement_reflns_used    6386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.47
_cell_volume                     1025.05(14)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14648
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.269
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0475 before and 0.0376 after correction.
The Ratio of minimum to maximum transmission is 0.9065.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       blocks
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.213
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.4289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4553
_reflns_number_total             5045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03929k2.cif
_cod_data_source_block           15lm_kumar_kks_99
_cod_depositor_comments
'Adding full bibliography for 7036928--7036933.cif.'
_cod_database_code               7036933
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C20(0.5) H20A(0.5) H20B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C6(H6A,H6B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C2(H2), C4(H4), C8(H8), C12(H12), C11(H11), C10(H10), C9(H9)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              80287
_olex2_submission_special_instructions 'No special instructions were received'