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_7055368
_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         'C17 H16 Br Cl P Pt0.5, C H2 Cl2'
_chemical_formula_sum            'C18 H18 Br Cl3 P Pt0.5'
_chemical_formula_weight         549.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-14
_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                103.369(4)
_cell_angle_beta                 106.943(3)
_cell_angle_gamma                107.517(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7628(3)
_cell_length_b                   11.1119(5)
_cell_length_c                   11.4634(5)
_cell_measurement_reflns_used    7545
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      76.0620
_cell_measurement_theta_min      4.2810
_cell_volume                     953.98(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      100.0(10)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -49.00   36.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -30.0000 85

  2 omega  -62.00   33.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   57.0000   60.0000 95

  3 omega -111.00  -16.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000 -180.0000 95

  4 omega   88.00  124.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000   30.0000 36

  5 omega   57.00  130.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000 -150.0000 73

  6 omega   34.00   60.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 26

  7 omega   39.00  113.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   90.0000 74

  8 omega   52.00  142.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   90.0000 90

  9 omega  108.00  137.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 29

 10 omega   44.00   71.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 27

 11 omega   32.00   61.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  120.0000 29

 12 omega   76.00  101.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  120.0000 25

 13 omega   62.00   88.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 26

 14 omega   84.00  109.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 25

 15 omega  127.00  168.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -90.0000 41

 16 omega   89.00  115.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -60.0000 26

 17 omega   82.00  108.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   30.0000 26

 18 omega   64.00  108.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -90.0000 44

 19 omega  107.00  149.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 42

 20 omega   44.00   92.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 48

 21 omega   39.00   64.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   30.0000 25

 22 omega   39.00   90.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 51

 23 omega   84.00  129.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -120.0000 45

 24 omega   38.00   82.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 44

 25 omega   88.00  151.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -150.0000 63

 26 omega   68.00  106.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 38

 27 omega  149.00  177.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -180.0000 28

 28 omega  102.00  128.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 26

 29 omega   60.00   92.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   90.0000 32

 30 omega  114.00  144.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -180.0000 30

 31 omega   91.00  142.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -71.0000 -106.5526 51

 32 omega   47.00   91.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 44

 33 omega   40.00   65.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -83.0000  -18.0000 25

 34 omega  109.00  135.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -83.0000  -18.0000 26

 35 omega   89.00  115.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -180.0000 26

 36 omega  126.00  151.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 25

 37 omega   34.00   61.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -180.0000 27

 38 omega  108.00  172.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -180.0000 64

 39 omega   47.00   72.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -71.0000 -106.5526 25

 40 omega    0.00   25.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       40.0000   94.0000  -49.5239 25

 41 omega  -60.00  -25.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000    0.0000 35

 42 omega -114.00  -64.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000    0.0000 50

 43 omega -113.00  -26.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  -90.0000 87

 44 omega    1.00   47.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       40.3787  -99.0000 -150.0000 46

 45 omega    9.00   34.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       44.0000   81.0000 -117.7837 25

 46 omega    6.00   31.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       44.0000   90.0000   80.7222 25

 47 omega   12.00   37.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       48.0000   84.0000  168.0649 25

 48 omega   18.00   43.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000   49.6074 25

 49 omega   19.00   44.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000  176.0149 25

 50 omega   27.00   53.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       60.0000   76.0000  -39.0357 26

 51 omega   32.00   64.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000  141.2482 32

 52 omega   32.00   58.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       64.0000   72.0000 -112.1865 26

 53 omega   35.00   61.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000 -163.1021 26

 54 omega   98.00  127.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000   39.2969 29

 55 omega   34.00   77.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -29.2138 43

 56 omega   35.00   66.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000   39.2969 31

 57 omega  112.00  144.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000  -85.8948 32

 58 omega   35.00   67.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000  -85.8948 32

 59 omega   41.00   80.00   1.0000    3.0600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000   80.9503 39

 60 omega   56.00   85.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -       84.0000   55.0000   63.8290 29

 61 omega   63.00   89.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -       92.0000   54.0000 -150.5907 26

 62 omega   66.00   92.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -       96.0000   62.0000  141.1123 26

 63 omega   79.00  168.00   1.0000   12.2400
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -30.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0451353000
_diffrn_orient_matrix_UB_12      -0.1396331000
_diffrn_orient_matrix_UB_13      -0.0967689000
_diffrn_orient_matrix_UB_21      0.0685162000
_diffrn_orient_matrix_UB_22      0.0672660000
_diffrn_orient_matrix_UB_23      -0.0881605000
_diffrn_orient_matrix_UB_31      0.1825364000
_diffrn_orient_matrix_UB_32      0.0075626000
_diffrn_orient_matrix_UB_33      0.0731333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.460
_diffrn_reflns_theta_min         4.303
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65101
_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_colour            colorless
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       prism
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0186P)^2^+0.4509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3481
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           kp1_new
_cod_depositor_comments
'Adding full bibliography for 7055365--7055370.cif.'
_cod_original_cell_volume        953.98(7)
_cod_original_formula_sum        'C18 H18 Br Cl3 P Pt0.50'
_cod_database_code               7055368
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Pt1 P2 C10 H20'
_reflns_odcompleteness_completeness 94.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_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
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C6(H6), C15(H15), C8(H8), C7(H7), C16(H16),
 C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              70662
_olex2_submission_special_instructions 'No special instructions were received'