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_7046518
_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         'C25 H28 Br N3 Pd'
_chemical_formula_sum            'C25 H28 Br N3 Pd'
_chemical_formula_weight         556.81
_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             2017-07-26
_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                 98.263(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9330(5)
_cell_length_b                   23.8367(10)
_cell_length_c                   18.1370(7)
_cell_measurement_reflns_used    6460
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      28.7810
_cell_measurement_theta_min      3.8020
_cell_volume                     4677.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      4.00  83.00   1.00    5.00    --   12.61  57.00-120.00   79
  2  \w    -35.00  13.00   1.00    5.00    --   12.61 -37.00 150.00   48
  3  \w    -16.00  84.00   1.00    5.00    --   12.61  57.00 -30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0322343000
_diffrn_orient_matrix_UB_12      0.0059233000
_diffrn_orient_matrix_UB_13      0.0359442000
_diffrn_orient_matrix_UB_21      -0.0562246000
_diffrn_orient_matrix_UB_22      -0.0017903000
_diffrn_orient_matrix_UB_23      0.0151324000
_diffrn_orient_matrix_UB_31      0.0099127000
_diffrn_orient_matrix_UB_32      -0.0290989000
_diffrn_orient_matrix_UB_33      0.0064039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0219P)^2^+3.3701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6869
_reflns_number_total             8678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01618f2.cif
_cod_data_source_block           20170721a
_cod_depositor_comments
'Adding full bibliography for 7046516--7046519.cif.'
_cod_database_code               7046518
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c1h1n1o1Cl1Pd1
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C23(H23), C39(H39), C48(H48)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C18(H18), C19(H19),
 C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
  C35(H35), C43(H43), C44(H44), C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              91265
_olex2_date_sample_data_collection 2017-07-21
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.727