On the mercuration, palladation, transmetalation and direct auration of a C^N^C pincer ligand.
McEllin, Alice Jane; Goult, Christopher A.; Whitwood, Adrian C.; Lynam, Jason M.; Bruce, Duncan W.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 872–876; doi:10.1039/d2dt04114f

data_7712105
_publ_section_title
;
 On the mercuration, palladation, transmetalation and direct auration of a
 C^N^C pincer ligand.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              872
_journal_page_last               876
_journal_paper_doi               10.1039/d2dt04114f
_journal_volume                  52
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H21 N O4'
_chemical_formula_sum            'C21 H21 N O4'
_chemical_formula_weight         351.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-05 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1230(5)
_cell_length_b                   14.4934(5)
_cell_length_c                   7.3773(3)
_cell_measurement_reflns_used    1939
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      70.7960
_cell_measurement_theta_min      5.1630
_cell_volume                     1830.83(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      109.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -21.00  69.00   1.00    1.00    --    0.00  57.00  60.00   90
  2  \w     27.00 111.00   1.00    3.00    --   54.00-125.00  60.00   84
  3  \w     33.00 123.00   1.00    3.00    --   54.00  57.00-120.00   90
  4  \w    -18.00  80.00   1.00    3.00    --   54.00 -37.00  60.00   98
  5  \w    103.00 178.00   1.00    3.00    --  108.00  77.00 -60.00   75
  6  \w     36.00 107.00   1.00    3.00    --  108.00 -91.00 -90.00   71
  7  \w    103.00 178.00   1.00    3.00    --  108.00  77.00-150.00   75
  8  \w     38.00 130.00   1.00    3.00    --  108.00 -50.00 -60.00   92
  9  \w     82.00 178.00   1.00    3.00    --  108.00  37.00 120.00   96
 10  \w    -44.00  73.00   1.00    1.00    --    0.00  19.00   0.00  117
 11  \w     33.00 123.00   1.00    3.00    --   54.00  57.00 150.00   90
 12  \w     28.00 126.00   1.00    3.00    --   54.00  37.00  60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225146000
_diffrn_orient_matrix_UB_12      -0.1019076000
_diffrn_orient_matrix_UB_13      -0.0280435000
_diffrn_orient_matrix_UB_21      -0.0863634000
_diffrn_orient_matrix_UB_22      0.0242874000
_diffrn_orient_matrix_UB_23      0.0335231000
_diffrn_orient_matrix_UB_31      -0.0110566000
_diffrn_orient_matrix_UB_32      0.0180004000
_diffrn_orient_matrix_UB_33      -0.2042862000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3595
_diffrn_reflns_point_group_measured_fraction_full 0.803
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        66.989
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         5.166
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       irregular
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and ethanol'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.126
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Flack x determined using 398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.26(12)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1318
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.478
_reflns_Friedel_fraction_full    0.569
_reflns_Friedel_fraction_max     0.569
_reflns_number_gt                1259
_reflns_number_total             1318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04114f2.cif
_cod_data_source_block           dwb1916
_cod_depositor_comments
'Adding full bibliography for 7712105--7712107.cif.'
_cod_original_cell_volume        1830.81(11)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7712105
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H21 N1 O4'
_chemical_oxdiff_usercomment     'Alice Jane McEllin AJM103'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              19984
_shelx_hkl_checksum              87909
_olex2_date_sample_data_collection 2019-11-26
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id AJM103
_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 1.230
_oxdiff_exptl_absorpt_empirical_full_min 0.851