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_7036929
_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 H33 N3 Pd S, C32 H12 B F24'
_chemical_formula_sum            'C57 H45 B F24 N3 Pd S'
_chemical_formula_weight         1377.23
_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
_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                 92.845(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9047(10)
_cell_length_b                   21.0538(15)
_cell_length_c                   21.9172(16)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.64
_cell_volume                     5947.4(8)
_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 1.000
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95309
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.580
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0630 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.9189.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       Block
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         14343
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0527P)^2^+8.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11508
_reflns_number_total             14343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03929k2.cif
_cod_data_source_block           15lm_kks60_new_3
_cod_depositor_comments
'Adding full bibliography for 7036928--7036933.cif.'
_cod_database_code               7036929
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.795
_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(F23) \\sim Ueq, Uanis(F14) \\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)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C14(H14), C20(H20), C29(H29), C31(H31), C49(H49), C43(H43), C39(H39), C41(H41),
  C27(H27), C45(H45), C47(H47), C33(H33), C35(H35), C37(H37)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              38393
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'