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_7701216
_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         'C21 H20 Cl I2 N3 O2 Pd'
_chemical_formula_sum            'C21 H20 Cl I2 N3 O2 Pd'
_chemical_formula_weight         742.05
_chemical_name_systematic
;
trans-(3-chloropyridyl)-1-(2-methoxyphenyoxy)methyl-3-methylbenzimidazol-2-ylidene palladium(II) iodide
;
_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     direct
_audit_creation_date             2019-03-22
_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                 93.4572(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6170(5)
_cell_length_b                   10.99476(3)
_cell_length_c                   15.82037(5)
_cell_measurement_reflns_used    32682
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.953
_cell_measurement_theta_min      1.2399
_cell_volume                     2364.25(9)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40488
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.452
_diffrn_source                   'Diamond Light Source'
_exptl_absorpt_coefficient_mu    3.335
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+1.6285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7258
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03400e2.cif
_cod_data_source_block           shelxt_a
_cod_depositor_comments
'Adding full bibliography for 7701214--7701219.cif.'
_cod_original_cell_volume        2364.24(9)
_cod_database_code               7701216
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.753
_shelx_estimated_absorpt_t_min   0.617
_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:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C17(H17), C3(H3), C4(H4), C18(H18), C11(H11), C10(H10),
 C19(H19), C16(H16), C12(H12), C9(H9)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'