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_7055365
_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 P'
_chemical_formula_sum            'C17 H16 Br P'
_chemical_formula_weight         331.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-15
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-09-21 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.0486(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3791(3)
_cell_length_b                   10.08862(14)
_cell_length_c                   15.5172(2)
_cell_measurement_reflns_used    17610
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.8610
_cell_measurement_theta_min      4.6100
_cell_volume                     2996.97(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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details
;
  1 omega   -8.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000   90.0000 40

  2 omega -114.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000   30.0000 103

  3 omega  -55.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000 -180.0000 42

  4 omega  -50.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -30.0000 82

  5 omega   68.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 40

  6 omega   36.00   66.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  150.0000 30

  7 omega   49.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 47

  8 omega   42.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 45

  9 omega   35.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 28

 10 omega   30.00   56.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  150.0000 26

 11 omega   93.00  149.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   30.0000 56

 12 omega   36.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 38

 13 omega   61.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  150.0000 43

 14 omega   52.00   78.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 26

 15 omega  146.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 26

 16 omega   76.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000 -150.0000 26

 17 omega   83.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 43

 18 omega   44.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   30.0000 50

 19 omega   56.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 42

 20 omega  114.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000   60.0000 26

 21 omega   60.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 36

 22 omega  142.00  167.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 25

 23 omega  137.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000   30.0000 35

 24 omega  105.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000   90.0000 45

 25 omega   46.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 45

 26 omega   51.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   60.0000 45

 27 omega  111.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 28

 28 omega  120.00  146.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  150.0000 26

 29 omega   41.00   66.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 25

 30 omega   70.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 26

 31 omega   91.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 25

 32 omega  103.00  129.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   12.0000   36.2361 26

 33 omega   52.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -60.0000 48

 34 omega  124.00  149.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -150.0000 25

 35 omega   92.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 26

 36 omega   47.00   72.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 25

 37 omega   64.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 25

 38 omega   44.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 25

 39 omega   62.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000    0.0000 26

 40 omega   32.00   60.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    9.0000  -55.0178 28

 41 omega   29.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000 -180.0000 50

 42 omega   36.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   12.0000   36.2361 49

 43 omega  -63.00  -37.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000 -120.0000 26

 44 omega -109.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  -90.0000 93

 45 omega -119.00  -83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000 -120.0000 36

 46 omega   68.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787   38.0000   90.0000 27

 47 omega   63.00   99.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000  150.0000 36

 48 omega   23.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787   38.0000   90.0000 27

 49 omega  101.00  127.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   17.0000 -171.7798 26

 50 omega   64.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   17.0000 -171.7798 27

 51 omega   77.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -48.0000   58.7825 25

 52 omega   55.00   81.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  -30.0000 26

 53 omega   65.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 35

 54 omega   81.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 26

 55 omega  127.00  153.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 26

 56 omega  103.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   90.0000 38

 57 omega   86.00  130.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   90.0000 44

 58 omega  123.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   -9.0000 -171.4549 27

 59 omega   80.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000   90.0000 37

 60 omega   79.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 42

 61 omega  148.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 26

 62 omega   89.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 6
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0020216000
_diffrn_orient_matrix_UB_12      0.0241353000
_diffrn_orient_matrix_UB_13      -0.0971031000
_diffrn_orient_matrix_UB_21      0.0501996000
_diffrn_orient_matrix_UB_22      -0.1181984000
_diffrn_orient_matrix_UB_23      0.0118601000
_diffrn_orient_matrix_UB_31      -0.0628458000
_diffrn_orient_matrix_UB_32      -0.0936143000
_diffrn_orient_matrix_UB_33      -0.0400562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38236
_diffrn_reflns_theta_full        76.35
_diffrn_reflns_theta_max         76.35
_diffrn_reflns_theta_min         4.62
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79972
_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    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.8964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                5769
_reflns_number_total             6269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           asb598
_cod_depositor_comments
;
Adding full bibliography for 7055365--7055370.cif

2017-03-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2996.96(8)
_cod_original_formula_moiety     '2(C17 H16 Br P)'
_cod_original_formula_sum        'C34 H32 Br2 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     662.36
_cod_database_code               7055365
_chemical_oxdiff_formula         'C18 P1 H25 Br1'
_reflns_odcompleteness_completeness 95.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95