Chiral Discrimination by A Binuclear Pd Complex Sensor using <sup>31</sup>P{<sup>1</sup>H} NMR.
Chen, Zhongxiang; Yang, Mingxue; Sun, Zhaofeng; Zhang, Xuebo; Xu, Jing; Bian, Guangling; Song, Ling; Analytical chemistry  (2019) –; doi:10.1021/acs.analchem.9b03661

data_1552765
_publ_section_title
;
 Chiral Discrimination by A Binuclear Pd Complex Sensor using
 <sup>31</sup>P{<sup>1</sup>H} NMR.
;
_journal_name_full               'Analytical chemistry'
_journal_paper_doi               10.1021/acs.analchem.9b03661
_journal_year                    2019
_chemical_formula_moiety         'C65 H52 N O P2 Pd, C H2 Cl2, B F4'
_chemical_formula_sum            'C66 H55 B Cl2 F4 N O P2 Pd'
_chemical_formula_weight         1204.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9362(4)
_cell_length_b                   20.2513(10)
_cell_length_c                   27.0124(15)
_cell_measurement_reflns_used    48011
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      59.6190
_cell_measurement_theta_min      2.3660
_cell_volume                     5982.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     34.00 111.00   0.50    0.37    --   75.22-109.00  31.00  154
  2  \w     91.00 118.00   0.50    0.37    --   75.22 109.00 126.00   54
  3  \w    -91.00 -48.00   0.50    0.37    --  -78.03 109.00 126.00   86
  4  \w   -128.00 -87.00   0.50    0.37    --  -78.03-109.00  31.00   82
  5  \w    -11.00  35.00   0.50    0.09    --   -1.41 -99.00  60.00   92
  6  \w    -74.00  28.00   0.50    0.09    --   -1.41 -77.00-120.00  204
  7  \w    -13.00  38.00   0.50    0.09    --   -1.41 -99.00-150.00  102
  8  \w    -26.00   2.00   0.50    0.09    --   14.00 101.00 -38.16   56
  9  \w    -23.00   2.00   0.50    0.09    --   18.00 102.00 -19.02   50
 10  \w    -18.00   7.00   0.50    0.09    --   22.00 100.00  38.00   50
 11  \w      3.00  36.00   0.50    0.09    --   34.00  86.00 108.76   66
 12  \w    -34.00  60.00   0.50    0.37    --   38.00 -58.00 -40.07  188
 13  \w      8.00  38.00   0.50    0.37    --   42.00  88.00  -0.23   60
 14  \w     13.00  38.00   0.50    0.37    --   46.00  86.00 -93.26   50
 15  \w     12.00  39.00   0.50    0.37    --   46.00  89.00-173.47   54
 16  \w     12.00  39.00   0.50    0.37    --   46.00  91.00  34.10   54
 17  \w    -43.00 -16.00   0.50    0.37    --  -50.00 -88.00-167.82   54
 18  \w    -44.00 -17.00   0.50    0.37    --  -50.00 -86.00 100.78   54
 19  \w    -44.00 -18.00   0.50    0.37    --  -54.00 -91.00 -76.50   52
 20  \w    -44.00 -18.00   0.50    0.37    --  -54.00 -91.00 167.26   52
 21  \w    -44.00 -18.00   0.50    0.37    --  -54.00 -91.00 -10.42   52
 22  \w     28.00  98.00   0.50    0.37    --   58.00  80.00 -29.78  140
 23  \w     27.00  57.00   0.50    0.37    --   58.00  82.00  42.07   60
 24  \w     30.00  70.00   0.50    0.37    --   62.00  84.00  75.27   80
 25  \w    -82.00 -34.00   0.50    0.37    --  -66.00 -83.00-157.90   96
 26  \w   -142.00-112.00   0.50    0.37    --  -70.00 -84.00   3.89   60
 27  \w    -87.00 -38.00   0.50    0.37    --  -70.00 -84.00   3.89   98
 28  \w    -65.00 -38.00   0.50    0.37    --  -70.00 -84.00 -80.68   54
 29  \w   -143.00 -93.00   0.50    0.37    --  -70.00 -84.00 -80.68  100
 30  \w    -97.00 -70.00   0.50    0.37    --  -70.00 -81.00  86.18   54
 31  \w    -64.00 -39.00   0.50    0.37    --  -70.00 -81.00  86.18   50
 32  \w   -139.00-113.00   0.50    0.37    --  -70.00 -81.00  86.18   52
 33  \w    -64.00 -38.00   0.50    0.37    --  -70.00 -84.00 129.32   52
 34  \w   -121.00 -94.00   0.50    0.37    --  -70.00 -84.00 129.32   54
 35  \w     44.00 147.00   0.50    0.37    --   74.00  79.00  -5.24  206
 36  \w   -117.00 -45.00   0.50    0.37    --  -74.00 -77.00  57.36  144
 37  \w    -91.00 -42.00   0.50    0.37    --  -74.00 -84.00-175.22   98
 38  \w   -129.00 -96.00   0.50    0.37    --  -74.00 -84.00-175.22   66
 39  \w    -86.00 -42.00   0.50    0.37    --  -74.00 -84.00-111.27   88
 40  \w   -140.00-101.00   0.50    0.37    --  -74.00 -84.00-111.27   78
 41  \w   -146.00 -43.00   0.50    0.37    --  -74.00 -82.00-101.36  206
 42  \w    -86.00 -42.00   0.50    0.37    --  -74.00 -83.00 156.45   88
 43  \w   -144.00 -87.00   0.50    0.37    --  -74.00 -83.00 156.45  114
 44  \w     38.00  98.00   0.50    0.37    --   75.22 -57.00  90.00  120
 45  \w      7.00  34.00   0.50    0.37    --   75.22 -57.00  90.00   54
 46  \w     62.00  92.00   0.50    0.37    --   75.22 -77.00 150.00   60
 47  \w      4.00  55.00   0.50    0.37    --   75.22 -77.00 150.00  102
 48  \w     22.00 101.00   0.50    0.37    --   75.22 -77.00-150.00  158
 49  \w     74.00 145.00   0.50    0.37    --   75.22 125.00  60.00  142
 50  \w    103.00 140.00   0.50    0.37    --   75.22 125.00-150.00   74
 51  \w     73.00  99.00   0.50    0.37    --   75.22 125.00-150.00   52
 52  \w      1.00 104.00   0.50    0.37    --   75.22 -77.00  30.00  206
 53  \w   -143.00 -46.00   0.50    0.37    --  -78.03 -84.00 -51.98  194
 54  \w   -107.00 -47.00   0.50    0.37    --  -78.03 -82.00 129.53  120
 55  \w   -149.00-123.00   0.50    0.37    --  -78.03 -82.00 129.53   52
 56  \w   -151.00 -49.00   0.50    0.37    --  -78.03 -78.00 -39.16  204
 57  \w    -93.00 -49.00   0.50    0.37    --  -78.03 -77.00-150.00   88
 58  \w    -31.00  -5.00   0.50    0.37    --  -78.03  57.00 -30.00   52
 59  \w   -152.00 -89.00   0.50    0.37    --  -78.03 -99.00  90.00  126
 60  \w   -112.00 -21.00   0.50    0.37    --  -78.03 125.00 -60.00  182
 61  \w   -147.00 -49.00   0.50    0.37    --  -78.03 -77.00  90.00  196
 62  \w    -94.00 -46.00   0.50    0.37    --  -78.03  57.00 -30.00   96
 63  \w   -138.00 -56.00   0.50    0.37    --  -78.03 -38.00 150.00  164
 64  \w    -79.00 -49.00   0.50    0.37    --  -78.03 -77.00  30.00   60
 65  \w   -150.00 -97.00   0.50    0.37    --  -78.03 -77.00  30.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0670323000
_diffrn_orient_matrix_UB_12      -0.0539057000
_diffrn_orient_matrix_UB_13      -0.0093993000
_diffrn_orient_matrix_UB_21      0.0101480000
_diffrn_orient_matrix_UB_22      0.0184317000
_diffrn_orient_matrix_UB_23      -0.0474890000
_diffrn_orient_matrix_UB_31      0.1018324000
_diffrn_orient_matrix_UB_32      0.0336923000
_diffrn_orient_matrix_UB_33      0.0109843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1351
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            129808
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        48.134
_diffrn_reflns_theta_max         48.134
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3166 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         8600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.1045
_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^)+(0.0708P)^2^+35.4987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8345
_reflns_number_total             8600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac9b03661_si_002.cif
_cod_data_source_block           exp_1362
_cod_database_code               1552765
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.946
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00X(H00X)
2.b Secondary CH2 refined with riding coordinates:
 N00A(H00A,H00B), C00M(H00C,H00D), C029(H02A,H02B)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00F(H00F), C00J(H00J), C00O(H00O), C00P(H00P), C00T(H00T),
 C00U(H00U), C00W(H00W), C00Y(H00Y), C010(H010), C011(H011), C014(H014),
 C015(H015), C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01D(H01D),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021),
 C023(H023), C024(H024), C025(H025), C026(H026), C027(H027)
;
_shelx_res_checksum              50186
_shelx_hkl_checksum              53836
_shelx_fab_checksum              95591
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.533
_oxdiff_exptl_absorpt_empirical_full_min 0.508