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_7036190
_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         'C12 H13 Br2 N3 Pd'
_chemical_formula_sum            'C12 H13 Br2 N3 Pd'
_chemical_formula_weight         465.47
_chemical_name_systematic        4b
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-19
_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                80.496(5)
_cell_angle_beta                 79.638(6)
_cell_angle_gamma                87.116(7)
_cell_formula_units_Z            2
_cell_length_a                   7.9713(7)
_cell_length_b                   9.1926(8)
_cell_length_c                   9.8150(4)
_cell_measurement_reflns_used    6257
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      30.3740
_cell_measurement_theta_min      3.3990
_cell_volume                     697.62(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -47.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -37.0000 -150.0000 27

  2 omega  -76.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000  -60.0000 76

  3 omega  -73.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000   90.0000 84

  4 omega  -80.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000 -150.0000 91

  5 omega  -66.00  -17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000   30.0000 49

  6 omega   20.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   19.0000   30.0000 42

  7 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000   90.0000 94

  8 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000 -150.0000 94

  9 omega  -39.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000    0.0000 77

 10 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000  -60.0000 94
;
_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      0.0271274000
_diffrn_orient_matrix_UB_12      -0.0716237000
_diffrn_orient_matrix_UB_13      -0.0137796000
_diffrn_orient_matrix_UB_21      0.0837400000
_diffrn_orient_matrix_UB_22      0.0143997000
_diffrn_orient_matrix_UB_23      0.0086063000
_diffrn_orient_matrix_UB_31      -0.0209248000
_diffrn_orient_matrix_UB_32      -0.0280365000
_diffrn_orient_matrix_UB_33      0.0726150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14130
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.043
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.670
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0331P)^2^+1.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                2945
_reflns_number_total             3472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02194d2.cif
_cod_data_source_block           mrc125_mo_a
_cod_depositor_comments
'Adding full bibliography for 7036182--7036191.cif.'
_cod_original_cell_volume        697.61(9)
_cod_database_code               7036190
_chemical_oxdiff_formula         'C24 H26 Br4 N6 Pd2'
_reflns_odcompleteness_completeness 99.88
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'