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_7701215
_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         '3(F6 P), C51 H51 N6 O6'
_chemical_formula_sum            'C51 H51 F18 N6 O6 P3'
_chemical_formula_weight         1278.89
_chemical_name_systematic
;
tris-methyl(methylbenzimidazol-1-yl)cyclotriguaiacylenyl hexafluorophosphate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-24
_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                75.410(11)
_cell_angle_beta                 80.946(12)
_cell_angle_gamma                78.773(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4847(9)
_cell_length_b                   16.4088(17)
_cell_length_c                   22.788(3)
_cell_measurement_reflns_used    586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.041
_cell_measurement_theta_min      1.9541
_cell_volume                     2639.3(6)
_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
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.1405
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8730
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        20.148
_diffrn_reflns_theta_max         20.148
_diffrn_reflns_theta_min         1.708
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9968
_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_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.2239
_refine_ls_R_factor_gt           0.1131
_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^)+(0.1937P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2906
_refine_ls_wR_factor_ref         0.3380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1834
_reflns_number_total             5085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03400e2.cif
_cod_data_source_block           mebzim
_cod_depositor_comments
'Adding full bibliography for 7701214--7701219.cif.'
_cod_database_code               7701215
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.994
_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. Restrained distances
 O6-C52
 1.43 with sigma of 0.02
 O6-C42
 1.43 with sigma of 0.02
 N1-C8
 1.34 with sigma of 0.02
 N2-C8
 1.34 with sigma of 0.02
3. Others
 Fixed Sof: N5(0.5) N7(0.5) C42(0.5) H42A(0.5) H42B(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C17(H17A,H17B), C25(H25A,H25B), C34(H34A,H34B), C42(H42A,H42B),
 C51(H51A,H51B), C52(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C19(H19),
 C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C36(H36), C39(H39),
  C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54)
4.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C33(H33A,H33B,
 H33C), C41(H41A,H41B,H41C), C49(H49A,H49B,H49C)
;
_olex2_submission_special_instructions 'No special instructions were received'