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_7036931
_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         'C25 H34 N3 Pd Se, C32 H12 B F24'
_chemical_formula_sum            'C57 H46 B F24 N3 Pd Se'
_chemical_formula_weight         1425.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-18
_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                90
_cell_angle_beta                 93.167(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.922(3)
_cell_length_b                   21.107(4)
_cell_length_c                   21.915(5)
_cell_measurement_reflns_used    3601
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.49
_cell_volume                     5968(2)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.948
_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  0.1013
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_laue_measured_fraction_full 0.959
_diffrn_reflns_laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47324
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.340
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0647 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.8800.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.152
_refine_diff_density_max         2.126
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         13654
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0904P)^2^+6.8812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7877
_reflns_number_total             13654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03929k2.cif
_cod_data_source_block           15lm_kks78
_cod_depositor_comments
'Adding full bibliography for 7036928--7036933.cif.'
_cod_database_code               7036931
_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. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F3) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C7(H7), C6(H6), C5(H5), C4(H4), C3(H3),
 C20(H20), C39(H39), C31(H31), C33(H33), C37(H37), C35(H35), C45(H45), C47(H47),
  C49(H49), C27(H27), C29(H29), C43(H43), C41(H41)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              39493
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'