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_7036930
_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         'C19 H22 N3 Pd S, C32 H12 B F24, 2(C4 H10 O)'
_chemical_formula_sum            'C59 H54 B F24 N3 O2 Pd S'
_chemical_formula_weight         1442.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-23
_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                 104.638(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.545(10)
_cell_length_b                   12.996(3)
_cell_length_c                   24.090(5)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.18
_cell_volume                     12584(5)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0663
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            112608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.647
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0633 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8938.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       Block
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.294
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         15192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0647P)^2^+70.5567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11593
_reflns_number_total             15192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03929k2.cif
_cod_data_source_block           15lm_kks91_a
_cod_depositor_comments
'Adding full bibliography for 7036928--7036933.cif.'
_cod_database_code               7036930
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.765
_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.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C8(H8A,H8B), C24(H24A,H24B), C26(H26A,H26B), C22(H22A,H22B),
 C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C16(H16), C4(H4), C6(H6), C2(H2), C3(H3),
 C5(H5), C41(H41), C57(H57), C33(H33), C31(H31), C55(H55), C53(H53), C45(H45),
 C39(H39), C37(H37), C49(H49), C47(H47), C29(H29)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              20822
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'