Amino acid-derived bisphenolate palladium complexes as C-C coupling catalysts
Fazekas, Eszter; Jenkins, David T.; Forbes, Andrew A.; Gallagher, Brendan; Rosair, Georgina; McIntosh, Ruaraidh D.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03068J

data_7708830
_publ_section_title
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 Amino acid-derived bisphenolate palladium complexes as C-C coupling
 catalysts
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03068J
_journal_year                    2021
_chemical_formula_moiety         'C23 H31 N O4'
_chemical_formula_sum            'C23 H31 N O4'
_chemical_formula_weight         385.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2021-03-16 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
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_cell_angle_alpha                70.3610(10)
_cell_angle_beta                 70.5070(10)
_cell_angle_gamma                76.5600(10)
_cell_formula_units_Z            4
_cell_length_a                   10.5479(2)
_cell_length_b                   14.5535(3)
_cell_length_c                   15.4442(3)
_cell_measurement_reflns_used    3876
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      50.90
_cell_measurement_theta_min      3.79
_cell_volume                     2085.52(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24899
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.563
_diffrn_reflns_theta_min         3.164
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.8374.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0729P)^2^+0.0723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5755
_reflns_number_total             8049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03068j2.cif
_cod_data_source_block           8v00160_0m
_cod_database_code               7708830
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.815
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C2'(H2')
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C7(H7a,H7b), C16(H16a,H16b), C5'(H5'a,H5'b), C7'(H7'a,H7'b),
 C16'(H16c,H16d)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C20(H20), C22(H22), C11'(H11'), C13'(H13'), C20'(H20'),
 C22'(H22')
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C6(H6a,H6b,H6c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c),
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C3'(H3'a,H3'b,H3'c), C6'(H6'a,H6'b,
 H6'c), C14'(H14d,H14e,H14f), C15'(H15d,H15e,H15f), C23'(H23d,H23e,H23f),
 C24'(H24d,H24e,H24f)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2a), O1'(H1'), O2'(H2'a)
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_shelx_res_checksum              77228
_olex2_submission_special_instructions 'No special instructions were received'