A palladacyclic N-heterocyclic carbene system used to probe the donating abilities of monoanionic chelators.
Yan, Xuechao; Feng, Rui; Yan, Chunhui; Lei, Peng; Guo, Shuai; Huynh, Han Vinh; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7830–7838; doi:10.1039/c8dt01618f

data_7046519
_publ_section_title
;
 A palladacyclic N-heterocyclic carbene system used to probe the donating
 abilities of monoanionic chelators.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7830
_journal_page_last               7838
_journal_paper_doi               10.1039/c8dt01618f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H39 Br2 N5 Pd'
_chemical_formula_sum            'C32 H39 Br2 N5 Pd'
_chemical_formula_weight         759.90
_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     dual
_audit_creation_date             2017-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.3500(3)
_cell_length_b                   8.65960(10)
_cell_length_c                   25.0145(2)
_cell_measurement_reflns_used    22369
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7080
_cell_measurement_theta_min      3.9060
_cell_volume                     6985.71(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  89.00   0.50    1.00    --    0.00  57.00 -30.00  222
  2  \w    -89.00  22.00   0.50    1.00    --    0.00 -57.00 -60.00  222
  3  \w    -89.00  18.00   0.50    1.00    --    0.00 -19.00-150.00  214
  4  \w     32.00 107.00   0.50    6.00    --   94.60 -30.00-120.00  150
  5  \w     37.00  63.00   0.50    6.00    --   94.60 -77.00-180.00   52
  6  \w     47.00  80.00   0.50    6.00    --   94.60 -30.00 150.00   66
  7  \w      5.00 115.00   0.50    6.00    --   94.60 -15.00 -30.00  220
  8  \w     74.00 123.00   0.50    6.00    --   94.60 -77.00-180.00   98
  9  \w     83.00 109.00   0.50    6.00    --   94.60  15.00 -90.00   52
 10  \w    146.00 177.00   0.50    6.00    --   94.60  15.00 -90.00   62
 11  \w     28.00 117.00   0.50    6.00    --   94.60 -61.00-180.00  178
 12  \w     10.00  36.00   0.50    6.00    --   94.60 -30.00 150.00   52
 13  \w      8.00 118.00   0.50    6.00    --   94.60 -15.00-150.00  220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0352614000
_diffrn_orient_matrix_UB_12      -0.0393903000
_diffrn_orient_matrix_UB_13      0.0428674000
_diffrn_orient_matrix_UB_21      0.0280047000
_diffrn_orient_matrix_UB_22      -0.0455909000
_diffrn_orient_matrix_UB_23      -0.0444545000
_diffrn_orient_matrix_UB_31      0.0159271000
_diffrn_orient_matrix_UB_32      0.1673860000
_diffrn_orient_matrix_UB_33      -0.0020531000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41137
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.908
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       needle
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.375
_refine_diff_density_min         -2.293
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         13750
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0981P)^2^+28.8836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12112
_reflns_number_total             13750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01618f2.cif
_cod_data_source_block           20170613-yxc-20
_cod_depositor_comments
'Adding full bibliography for 7046516--7046519.cif.'
_cod_database_code               7046519
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Pd C H N Br'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C46') \\sim Ueq, Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq,
Uanis(C49') \\sim Ueq, Uanis(C50') \\sim Ueq, Uanis(C51') \\sim Ueq, Uanis(C52)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Same fragment restrains
{C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as
{C34, C35, C36, C37, C38}
4. Others
 Fixed Sof: H45A(0.5) H45B(0.5) H45C(0.5) H45D(0.5) C46(0.5) C47(0.5) H47(0.5)
 C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5)
 C46'(0.5) C47'(0.5) H47'(0.5) C48'(0.5) H48'(0.5) C49'(0.5) H49'(0.5)
 C50'(0.5) H50'(0.5) C51'(0.5) H51'(0.5)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C30(H30), C53(H53), C62(H62)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C13(H13A,H13B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C45(H45A,H45B), C45(H45C,H45D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C25(H25), C26(H26), C27(H27), C28(H28), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C47'(H47'), C48'(H48'), C49'(H49'), C50'(H50'), C51'(H51'), C57(H57),
  C58(H58), C59(H59), C60(H60)
5.d Fitted hexagon refined as free rotating group:
 C39(C40,C41,C42,C43,C44), C46(C47,C48,C49,C50,C51), C46'(C47',C48',C49',C50',
 C51')
5.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              9922
_shelx_fab_checksum              39441
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.138
_oxdiff_exptl_absorpt_empirical_full_min 0.354