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_7036191
_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 H26 N8 Pd, C2 H6 O S, 2(Br)'
_chemical_formula_sum            'C32 H32 Br2 N8 O Pd S'
_chemical_formula_weight         842.94
_chemical_name_systematic        6f
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_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                 107.066(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.370(4)
_cell_length_b                   12.2010(19)
_cell_length_c                   18.606(2)
_cell_measurement_reflns_used    2743
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      24.1970
_cell_measurement_theta_min      3.6350
_cell_volume                     6590.8(16)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -25.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -57.0000  -30.0000 28

  2 omega  -22.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -57.0000  -90.0000 58

  3 omega  -30.00    8.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -63.0000 -110.3798 38

  4 omega  -78.00  -14.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000 -150.0000 64

  5 omega   -5.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072   37.0000   90.0000 82
;
_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      0.0217878000
_diffrn_orient_matrix_UB_12      -0.0244417000
_diffrn_orient_matrix_UB_13      0.0032144000
_diffrn_orient_matrix_UB_21      0.0096947000
_diffrn_orient_matrix_UB_22      0.0526414000
_diffrn_orient_matrix_UB_23      -0.0003651000
_diffrn_orient_matrix_UB_31      0.0055530000
_diffrn_orient_matrix_UB_32      0.0025653000
_diffrn_orient_matrix_UB_33      0.0396804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23167
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.741
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.464
_refine_diff_density_min         -2.792
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+75.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                4905
_reflns_number_total             8170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02194d2.cif
_cod_data_source_block           mrc147_mo
_cod_depositor_comments
'Adding full bibliography for 7036182--7036191.cif.'
_cod_original_cell_volume        6590.9(16)
_cod_database_code               7036191
_chemical_oxdiff_formula         'C256 H256 Br16 N64 O8 Pd8 S8'
_reflns_odcompleteness_completeness 99.70
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H21A(0.5) H21B(0.5) H21C(0.5) H21D(0.5) N5B(0.5) C16B(0.5)
 H16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) H18B(0.5) C19B(0.5) H19B(0.5)
 C20B(0.5) N5A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C18A(0.5) H18A(0.5)
 C19A(0.5) H19A(0.5) C20A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C21(H21A,H21B), C21(H21C,H21D), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'