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_7055369
_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 Pt'
_chemical_formula_sum            'C34 H34 Cl2 P2 Pt'
_chemical_formula_weight         770.54
_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                 100.854(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9317(6)
_cell_length_b                   15.5172(6)
_cell_length_c                   16.9442(8)
_cell_measurement_reflns_used    5617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5810
_cell_measurement_theta_min      3.8180
_cell_volume                     3081.0(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -67.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2537  -57.0000   90.0000 50

  2 omega -112.00  -86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2537  -57.0000   90.0000 26

  3 omega  -49.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2537   38.0000 -120.0000 85

  4 omega  -38.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2537   38.0000  -30.0000 57

  5 omega    7.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2537  -99.0000   30.0000 44

  6 omega  126.00  157.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 31

  7 omega   54.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 34

  8 omega   90.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -90.0000 86

  9 omega  126.00  167.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -120.0000 41

 10 omega   99.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 27

 11 omega   34.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  120.0000 42

 12 omega   80.00  145.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  120.0000 65

 13 omega  149.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 28

 14 omega   62.00  146.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  120.0000 84

 15 omega   42.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 40

 16 omega  140.00  167.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 27

 17 omega   81.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 25

 18 omega   35.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 43

 19 omega   29.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  120.0000 48

 20 omega   39.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 54

 21 omega   30.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000    0.0000 39

 22 omega  111.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000    0.0000 28

 23 omega   61.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -120.0000 29

 24 omega  105.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -120.0000 45

 25 omega   49.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 25

 26 omega  114.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000 -150.0000 61

 27 omega   74.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 25

 28 omega  126.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000   30.0000 25

 29 omega   35.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 51
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1088671000
_diffrn_orient_matrix_UB_12      0.0477311000
_diffrn_orient_matrix_UB_13      0.0118488000
_diffrn_orient_matrix_UB_21      0.0654574000
_diffrn_orient_matrix_UB_22      0.0395738000
_diffrn_orient_matrix_UB_23      0.0787196000
_diffrn_orient_matrix_UB_31      0.0336364000
_diffrn_orient_matrix_UB_32      0.0775935000
_diffrn_orient_matrix_UB_33      -0.0472149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20759
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.998
_diffrn_reflns_theta_min         3.895
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.258
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            less
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1042
_exptl_crystal_size_mid          0.0925
_exptl_crystal_size_min          0.0773
_refine_diff_density_max         3.985
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0557
_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^)+(0.1045P)^2^+3.3475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4572
_reflns_number_total             5834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           kp3
_cod_depositor_comments
'Adding full bibliography for 7055365--7055370.cif.'
_cod_database_code               7055369
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C34 H34 Cl2 P2 Pt'
_reflns_odcompleteness_completeness 94.11
_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:
 C2A(H2A), C8A(H8A), C3(H3), C12A(H12A), C2(H2), C5A(H5A), C16A(H16A), C8(H8),
 C3A(H3A), C7A(H7A), C6A(H6A), C13A(H13A), C14A(H14A), C15A(H15A), C7(H7),
 C6(H6), C5(H5), C16(H16), C12(H12), C15(H15), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18A(H18A,H18B,H18C), C18(H18D,
 H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'