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_1552764
_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_absolute_configuration rmad
_chemical_formula_moiety         'C52 H41 N2 O P2 Pd, 2(B F4), C6 H16 N'
_chemical_formula_sum            'C58 H57 B2 F8 N3 O P2 Pd'
_chemical_formula_weight         1154.02
_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   mixed
_audit_creation_date             2019-07-01
_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                   10.649(4)
_cell_length_b                   14.860(7)
_cell_length_c                   32.973(12)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.248
_cell_measurement_theta_min      2.356
_cell_volume                     5218(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            50799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.265
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0892 before and 0.0653 after correction. The Ratio of minimum to maximum transmission is 0.8477. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 4304 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         12893
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.6126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11274
_reflns_number_total             12893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac9b03661_si_001.cif
_cod_data_source_block           mo_19040901_0m_a
_cod_original_cell_volume        5218(3)
_cod_database_code               1552764
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C01N, C01{, C0, C0AA, C1AA, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01M, C01Z, C023, C01X, C01Y, C022
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F1)=Sof(F2)=Sof(F1AA)=Sof(F2AA)=1-FVAR(1)
 Sof(F3)=Sof(F5)=Sof(F6)=Sof(F0AA)=FVAR(1)
 Sof(H01D)=Sof(C01N)=Sof(C01{)=Sof(H01{)=Sof(C0)=Sof(H0)=Sof(C0AA)=Sof(H0AA)=
 Sof(C1AA)=Sof(H1AA)=Sof(C1)=Sof(H1)=1-FVAR(2)
 Sof(H01G)=Sof(C01M)=Sof(C01Z)=Sof(H01Z)=Sof(C023)=Sof(H023)=Sof(C01X)=
 Sof(H01X)=Sof(C01Y)=Sof(H01Y)=Sof(C022)=Sof(H022)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C01G(H01G), C01G(H01D), N1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 N008(H00A,H00B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C00B(H00C), C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I), C00J(H00J),
 C00Q(H00Q), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C014(H014),
 C015(H015), C016(H016), C017(H017), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01Z(H01Z), C023(H023), C01X(H01X), C01Y(H01Y),
 C022(H022), C01{(H01{), C0(H0), C0AA(H0AA), C1AA(H1AA), C1(H1)
4.d Fitted hexagon refined as free rotating group:
 C01M(C01Z,C023,C01X,C01Y,C022)
4.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              28910
_shelx_hkl_checksum              3003
_olex2_submission_special_instructions 'No special instructions were received'