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_7055366
_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 H32 Br2 Cl2 P2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H36 Br2 Cl6 P2 Pd'
_chemical_formula_weight         1009.51
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-13
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-10-20 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                103.246(5)
_cell_angle_beta                 106.855(5)
_cell_angle_gamma                107.784(5)
_cell_formula_units_Z            1
_cell_length_a                   8.7824(4)
_cell_length_b                   11.1066(6)
_cell_length_c                   11.4473(6)
_cell_measurement_reflns_used    3299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2377
_cell_measurement_theta_min      2.6162
_cell_volume                     953.73(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.9828
_diffrn_measured_fraction_theta_max 0.9828
_diffrn_measurement_details
;
  1 omega  -29.00    2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   57.0000 -180.0000 31

  2 omega  -79.00  -53.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -178.0000  -90.0000 26

  3 omega  -24.00   22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000    0.0000 46

  4 omega  -19.00   14.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000 -150.0000 33

  5 omega   50.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152 -178.0000 -180.0000 45

  6 omega   36.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  178.0000 -150.0000 31

  7 omega   -7.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   38.0000    0.0000 94

  8 omega  -39.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -19.0000  150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0235843000
_diffrn_orient_matrix_UB_12      0.0031092000
_diffrn_orient_matrix_UB_13      -0.0636332000
_diffrn_orient_matrix_UB_21      0.0852437000
_diffrn_orient_matrix_UB_22      0.0476322000
_diffrn_orient_matrix_UB_23      0.0174643000
_diffrn_orient_matrix_UB_31      0.0254719000
_diffrn_orient_matrix_UB_32      -0.0533098000
_diffrn_orient_matrix_UB_33      -0.0204318000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7578
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tables
_exptl_crystal_F_000             500
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.650
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+1.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                3390
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           km868
_cod_depositor_comments
'Adding full bibliography for 7055365--7055370.cif.'
_cod_original_cell_volume        953.72(9)
_cod_database_code               7055366
_chemical_oxdiff_formula         'pt1 C15 N4 Cl2'
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32