Synthesis of a series of new platinum organometallic complexes derived from bidentate Schiff-base ligands and their catalytic activity in the hydrosilylation and dehydrosilylation of styrene.
Lachachi, M. Belhadj; Benabdallah, Tayeb; Aguiar, Pedro M.; Youcef, M. Hadj; Whitwood, Adrian C.; Lynam, Jason M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11919–11928; doi:10.1039/c5dt01407g

data_7035401
_publ_section_title
;
 Synthesis of a series of new platinum organometallic complexes derived
 from bidentate Schiff-base ligands and their catalytic activity in the
 hydrosilylation and dehydrosilylation of styrene.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11919
_journal_page_last               11928
_journal_paper_doi               10.1039/c5dt01407g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C52 H52 N2 O5 Pt2, 0.5(C5 H12)'
_chemical_formula_sum            'C54.5 H58 N2 O5 Pt2'
_chemical_formula_weight         1211.21
_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
_audit_creation_date             2014-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4957)
;
_audit_update_record
;
2015-03-20 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                87.663(3)
_cell_angle_beta                 84.731(4)
_cell_angle_gamma                82.141(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1629(4)
_cell_length_b                   17.1325(7)
_cell_length_c                   19.9614(8)
_cell_measurement_reflns_used    6720
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      30.0220
_cell_measurement_theta_min      3.2600
_cell_volume                     2415.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_details
;
  1 omega    3.00   30.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5455   57.0000    0.0000 27

  2 omega   -7.00   91.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5455   77.0000  120.0000 98

  3 omega   22.00   63.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5455  -99.0000 -120.0000 41

  4 omega  -45.00   52.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5455  -77.0000    0.0000 97

  5 omega  -17.00   88.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5455   19.0000  -60.0000 105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0066223000
_diffrn_orient_matrix_UB_12      -0.0330855000
_diffrn_orient_matrix_UB_13      0.0226178000
_diffrn_orient_matrix_UB_21      -0.0859821000
_diffrn_orient_matrix_UB_22      -0.0100514000
_diffrn_orient_matrix_UB_23      -0.0099919000
_diffrn_orient_matrix_UB_31      0.0513068000
_diffrn_orient_matrix_UB_32      -0.0235038000
_diffrn_orient_matrix_UB_33      -0.0257491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19471
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.136
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.835
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.3379
_exptl_crystal_size_mid          0.1045
_exptl_crystal_size_min          0.0492
_refine_diff_density_max         2.454
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         12298
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9469
_reflns_number_total             12298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01407g2.cif
_cod_data_source_block           '[6e]'
_cod_depositor_comments
'Adding full bibliography for 7035397--7035401.cif.'
_cod_original_cell_volume        2415.37(18)
_cod_original_formula_sum        'C54.50 H58 N2 O5 Pt2'
_cod_database_code               7035401
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H24 N1 O3 Pt1'
_chemical_oxdiff_usercomment     'Billy's PtL5COD'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) = Uanis(C57)
3. Others
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) C57(0.5)
 H57A(0.5) H57B(0.5) H57C(0.5)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30), C31(H31), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,
 H28B), C29(H29A,H29B), C32(H32A,H32B), C33(H33A,H33B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
  C45(H45), C47(H47), C48(H48), C50(H50), C51(H51)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C57(H57A,H57B,
 H57C)
;
_olex2_date_sample_data_collection 2014-04-23
_olex2_date_sample_submission    1396911600
_olex2_exptl_crystal_mounting_method 'oil on loop'
_olex2_submission_special_instructions 'No special instructions were received'