1,4-Dihydrophosphinolines and their complexes with group 10 metals
Klingenberg, Margarita A.; Bogachenkov, Alexander S.; Kinzhalov, Mikhail A.; Vasilyev, Aleksander V.; Boyarskiy, Vadim P.; New J. Chem. 40 (2016) 3336–; doi:10.1039/C5NJ03038B

data_7055370
_publ_section_title
;
 1,4-Dihydrophosphinolines and their complexes with group 10 metals
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              3336
_journal_paper_doi               10.1039/C5NJ03038B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C34 H34 Cl2 P2 Pd'
_chemical_formula_sum            'C34 H34 Cl2 P2 Pd'
_chemical_formula_weight         681.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-20 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.105(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2369(4)
_cell_length_b                   8.2187(2)
_cell_length_c                   15.0367(5)
_cell_measurement_reflns_used    6692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8990
_cell_measurement_theta_min      4.5980
_cell_volume                     1511.98(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -102.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  120.0000 67

  2 omega -106.00  -80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787 -142.0000 -167.0000 26

  3 omega  -46.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -60.0000 81

  4 omega  -50.00   17.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -120.0000 67

  5 omega  -76.00   37.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   83.0000    9.0000 113

  6 omega   90.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000  -60.0000 31

  7 omega   62.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000 -120.0000 67

  8 omega   72.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000    0.0000 26

  9 omega  109.00  146.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 37

 10 omega   57.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  120.0000 74

 11 omega  117.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 26

 12 omega   37.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 52

 13 omega   50.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 55

 14 omega  151.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 26

 15 omega   86.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -120.0000 32

 16 omega  119.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 26

 17 omega   65.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 26

 18 omega   67.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 39

 19 omega   94.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 53

 20 omega   97.00  172.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 75

 21 omega   89.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -30.0000 27

 22 omega   75.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 33

 23 omega  127.00  153.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  120.0000 26

 24 omega   84.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 91

 25 omega   63.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 29

 26 omega   45.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -60.0000 32

 27 omega  136.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  120.0000 38

 28 omega   90.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 26

 29 omega   68.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 43

 30 omega   74.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 25

 31 omega   80.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000    0.0000 35

 32 omega   86.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   60.0000 25

 33 omega   95.00  136.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 41

 34 omega  103.00  129.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000   60.0000 26

 35 omega   85.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -30.0000 64

 36 omega   87.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 25

 37 omega  140.00  166.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 26

 38 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 27

 39 omega   41.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000    0.0000 32

 40 omega   31.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -120.0000 72

 41 omega   38.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 26

 42 omega   36.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 46

 43 omega   46.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -150.0000 25

 44 omega   63.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -180.0000 27

 45 omega  138.00  164.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 26

 46 omega   86.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 25

 47 omega  138.00  163.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 25

 48 omega   68.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -90.0000 26

 49 omega  105.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  -90.0000 29

 50 omega   62.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000   90.0000 51

 51 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0453812000
_diffrn_orient_matrix_UB_12      0.1027081000
_diffrn_orient_matrix_UB_13      0.0780667000
_diffrn_orient_matrix_UB_21      -0.0423402000
_diffrn_orient_matrix_UB_22      -0.1273421000
_diffrn_orient_matrix_UB_23      0.0661989000
_diffrn_orient_matrix_UB_31      0.1095259000
_diffrn_orient_matrix_UB_32      -0.0916245000
_diffrn_orient_matrix_UB_33      -0.0046074000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18145
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.214
_diffrn_reflns_theta_min         4.616
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0344P)^2^+3.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2860
_reflns_number_total             3166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           kp_4
_cod_depositor_comments
'Adding full bibliography for 7055365--7055370.cif.'
_cod_database_code               7055370
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Pt C10 H10 N2 O2'
_reflns_odcompleteness_completeness 95.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C3(H3), C2(H2), C15(H15), C14(H14), C12(H12), C8(H8), C13(H13),
 C7(H7), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'