Rapid interconversion of diastereomers of [PdCl{P(OC6H4NMe)2}{P(OC6H4NMe)OC6H4NHMe}]
Carroll, Hannah K.; Brown, Matthew L.; Yap, Vanessa C.; Magnuson, Justine R.; Reich, Noah A.J.; Macdonald, Alexander G.P.; Montgomery, Craig D.; Inorganica Chimica Acta 501 (2020) 119239–; doi:10.1016/j.ica.2019.119239

data_1565600
_publ_section_title
;
 Rapid interconversion of diastereomers of
 [PdCl{P(OC6H4NMe)2}{P(OC6H4NMe)OC6H4NHMe}]
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119239
_journal_paper_doi               10.1016/j.ica.2019.119239
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C28 H29 Cl N4 O4 P2 Pd'
_chemical_formula_sum            'C28 H29 Cl N4 O4 P2 Pd'
_chemical_formula_weight         689.34
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                97.753(5)
_cell_angle_beta                 112.821(5)
_cell_angle_gamma                95.185(5)
_cell_formula_units_Z            4
_cell_length_a                   13.4859(8)
_cell_length_b                   13.9193(8)
_cell_length_c                   16.7686(10)
_cell_measurement_reflns_used    7497
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.76
_cell_measurement_theta_min      2.909
_cell_volume                     2839.5(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2018.1-0'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics
;
ShelxLe (H\:ubschle, 2011), Olex2 (Dolomanov et al., 2009)'
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1446
_diffrn_reflns_Laue_measured_fraction_full 0.878
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10938
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        67.201
_diffrn_reflns_theta_max         67.201
_diffrn_reflns_theta_min         2.909
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.557
_exptl_absorpt_correction_T_max  0.752818
_exptl_absorpt_correction_T_min  0.461690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 5 output contains 38763 reflections, 
Rint = 0.1024  for all   19590  observations and
 Rint = 0.0472  for all    2224  observations with I > 3sigma(I)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1:1 THF/hexanes'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.205
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         10938
_refine_ls_number_restraints     777
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1148P)^2^+13.6919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6492
_reflns_number_total             10938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-501-119239.cif
_cod_data_source_block           1
_cod_database_code               1565600
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.519
_exptl_absorpt_special_details
;
HKLF 5 dataset constructed from all observed data
Reflections merged according to point-group -1    
Single reflections that also occur in composites not omitted
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.186(15) 0.14(2) 0.16(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-H2
 0.87 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N7) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.003
Uanis(C48) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.003
Uanis(C42) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.003
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
6.a Ternary CH refined with riding coordinates:
 N6(H6)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C16(H16), C19(H19), C18(H18), C23(H23), C26(H26), C25(H25), C24(H24),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C)
;
_shelx_res_checksum              19434
_shelx_hkl_checksum              16056
_olex2_submission_special_instructions 'No special instructions were received'