Solid-state structure, solution-state behaviour and catalytic activity of electronically divergent C,N-chelating palladium-N-heterocyclic carbene complexes.
Chapman, Michael R.; Lake, Benjamin R. M.; Pask, Christopher M.; Nguyen, Bao N.; Willans, Charlotte E.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15938–15948; doi:10.1039/c5dt02194d

data_7036188
_publ_section_title
;
 Solid-state structure, solution-state behaviour and catalytic activity of
 electronically divergent C,N-chelating palladium-N-heterocyclic carbene
 complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15938
_journal_page_last               15948
_journal_paper_doi               10.1039/c5dt02194d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H28 N8 Pd, 2(F6 P)'
_chemical_formula_sum            'C30 H28 F12 N8 P2 Pd'
_chemical_formula_weight         896.94
_chemical_name_systematic        7f
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.704(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0821(4)
_cell_length_b                   20.5140(10)
_cell_length_c                   20.6555(9)
_cell_measurement_reflns_used    4655
_cell_measurement_temperature    119.99(13)
_cell_measurement_theta_max      24.7990
_cell_measurement_theta_min      3.3970
_cell_volume                     3401.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   31.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   30.0000 28

  2 omega   -6.00   80.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000 -150.0000 86

  3 omega  -20.00   16.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -150.0000 36

  4 omega   54.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000   60.0000 29

  5 omega  -27.00   32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000   60.0000 59

  6 omega  -28.00   24.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000  120.0000 52

  7 omega   11.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000    0.0000 25

  8 omega   -8.00   17.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0278782000
_diffrn_orient_matrix_UB_12      -0.0279914000
_diffrn_orient_matrix_UB_13      -0.0157337000
_diffrn_orient_matrix_UB_21      0.0631823000
_diffrn_orient_matrix_UB_22      0.0188787000
_diffrn_orient_matrix_UB_23      -0.0121039000
_diffrn_orient_matrix_UB_31      0.0551026000
_diffrn_orient_matrix_UB_32      -0.0074802000
_diffrn_orient_matrix_UB_33      0.0283122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31660
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8440
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+16.5313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                5822
_reflns_number_total             8440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02194d2.cif
_cod_data_source_block           mrc100_mo
_cod_depositor_comments
'Adding full bibliography for 7036182--7036191.cif.'
_cod_database_code               7036188
_chemical_oxdiff_formula         'C120 H112 F48 N32 P8 Pd4'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-F10B = P2-F7A = P2-F7B = P2-F8A = P2-F8B = P2-F9A = P2-F9B = P2-F10A
 1.58 with sigma of 0.01
 F9A-F10A
 2.25 with sigma of 0.02
 F10A-F7A
 2.25 with sigma of 0.02
 F7A-F8A
 2.25 with sigma of 0.02
 F8A-F9A
 2.25 with sigma of 0.02
 F9B-F10B
 2.25 with sigma of 0.02
 F10B-F7B
 2.25 with sigma of 0.02
 F7B-F8B
 2.25 with sigma of 0.02
 F8B-F9B
 2.25 with sigma of 0.02
3. Others
 Fixed Sof: F9A(0.7) F10A(0.7) F7A(0.7) F8A(0.7) F7B(0.3) F8B(0.3) F10B(0.3)
 F9B(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C10(H10A,H10B), C21(H21A,H21B), C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C2(H2), C9(H9), C18(H18), C8(H8), C27(H27), C16(H16),
 C17(H17), C19(H19), C4(H4), C28(H28), C23(H23), C1(H1), C24(H24), C13(H13),
 C3(H3), C30(H30), C29(H29), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'