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_7055367
_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 Pt'
_chemical_formula_sum            'C34 H32 Br2 Cl2 P2 Pt'
_chemical_formula_weight         928.34
_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             2015-10-15
_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                 109.582(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3816(3)
_cell_length_b                   18.9270(4)
_cell_length_c                   16.0478(4)
_cell_measurement_reflns_used    15705
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      36.1320
_cell_measurement_theta_min      3.1980
_cell_volume                     3257.07(15)
_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      100.00(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -110.00  -54.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -      -35.2878  178.0000   60.0000 56

  2 omega   12.00   37.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -      -35.2878   38.0000 -120.0000 25

  3 omega  -60.00   -2.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -      -35.2878   38.0000 -120.0000 58

  4 omega   36.00  106.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -       36.5378  178.0000    0.0000 70

  5 omega   36.00  111.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -       36.5378  178.0000   90.0000 75

  6 omega   35.00  103.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -       36.5378  178.0000  150.0000 68

  7 omega -102.00  -63.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -      -35.2878  -38.0000   90.0000 39

  8 omega  -58.00  -33.00   1.0000   70.9200
omega____ theta____ kappa____ phi______ frames
    -      -35.2878  -57.0000   30.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0592733000
_diffrn_orient_matrix_UB_12      -0.0072110000
_diffrn_orient_matrix_UB_13      0.0318286000
_diffrn_orient_matrix_UB_21      -0.0245390000
_diffrn_orient_matrix_UB_22      -0.0306910000
_diffrn_orient_matrix_UB_23      0.0134814000
_diffrn_orient_matrix_UB_31      0.0161077000
_diffrn_orient_matrix_UB_32      -0.0202407000
_diffrn_orient_matrix_UB_33      -0.0317671000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25858
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41292
_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            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       needle
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.773
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.110
_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     374
_refine_ls_number_reflns         7480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+7.3258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6829
_reflns_number_total             7480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03038b2.cif
_cod_data_source_block           103-121-2746_kma-805
_cod_depositor_comments
'Adding full bibliography for 7055365--7055370.cif.'
_cod_original_cell_volume        3257.08(15)
_cod_database_code               7055367
_chemical_oxdiff_formula         'Pt P2 Cl2 Br2 C22 H22'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.02
_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:
 C3A(H3A), C8A(H8A), C16A(H16A), C16(H16), C14(H14), C13(H13), C15A(H15A),
 C14A(H14A), C15(H15), C12A(H12A), C7A(H7A), C12(H12), C3(H3), C5A(H5A),
 C13A(H13A), C5(H5), C6A(H6A), C8(H8), C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C18(H18D,H18E,H18F), C17A(H17D,
 H17E,H17F)
;
_shelx_res_checksum              50916
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'