Cyclotriveratrylene-tethered trinuclear palladium(ii)-NHC complexes; reversal of site selectivity in Suzuki-Miyaura reactions.
Fowler, Jonathan M.; Britton, Edward; Pask, Christopher M.; Willans, Charlotte E.; Hardie, Michaele J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14687–14695; doi:10.1039/c9dt03400e

data_7701219
_publ_section_title
;
 Cyclotriveratrylene-tethered trinuclear palladium(ii)-NHC complexes;
 reversal of site selectivity in Suzuki-Miyaura reactions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14687
_journal_page_last               14695
_journal_paper_doi               10.1039/c9dt03400e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C27 H24 Cl I2 N3 O2 Pd)'
_chemical_formula_sum            'C54 H48 Cl2 I4 N6 O4 Pd2'
_chemical_formula_weight         1636.28
_chemical_name_systematic
;
trans-(3-chloropyridyl)-1-(2-methoxyphenyoxy)methyl-3-benzyllbenzimidazol-2-ylidene palladium(II) iodide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.02430(10)
_cell_length_b                   14.5623(2)
_cell_length_c                   35.8034(5)
_cell_measurement_reflns_used    21345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      1.10
_cell_volume                     5685.58(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            74794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.502
_diffrn_reflns_theta_min         1.115
_diffrn_source                   'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    2.783
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9872
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.048: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       needle
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         11597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+11.1322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7865
_reflns_number_total             11597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03400e2.cif
_cod_data_source_block           shelxt_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7701214--7701219.cif.'
_cod_database_code               7701219
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.788
_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:
 C2(H2A,H2B), C29(H29A,H29B), C42(H42A,H42B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C13(H13), C40(H40), C50(H50), C39(H39), C12(H12), C10(H10), C4(H4),
 C37(H37), C52(H52), C54(H54), C27(H27), C26(H26), C38(H38), C31(H31), C53(H53),
  C11(H11), C25(H25), C47(H47), C20(H20), C44(H44), C35(H35), C19(H19),
 C45(H45), C46(H46), C32(H32), C17(H17), C7(H7), C6(H6), C8(H8), C33(H33),
 C18(H18), C5(H5), C34(H34)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C49(H49A,H49B,H49C)
;
_olex2_submission_special_instructions 'No special instructions were received'