Platinum macrocatalyst for heterogeneous Si-O dehydrocoupling.
Deriabin, Konstantin V.; Golovenko, Ekaterina A.; Antonov, Nikita S.; Baykov, Sergey V.; Boyarskiy, Vadim P.; Islamova, Regina M.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00651d

data_7712882
_publ_section_title
;
 Platinum macrocatalyst for heterogeneous Si-O dehydrocoupling.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00651d
_journal_year                    2023
_chemical_formula_moiety         'C34 H32 Cl N5 O2 Pt, 2(C3 F3)'
_chemical_formula_sum            'C40 H32 Cl F6 N5 O2 Pt'
_chemical_formula_weight         959.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-22 deposited with the CCDC.	2023-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                107.1440(10)
_cell_angle_beta                 103.5320(10)
_cell_angle_gamma                92.7200(10)
_cell_formula_units_Z            2
_cell_length_a                   8.54280(10)
_cell_length_b                   14.88440(10)
_cell_length_c                   15.92190(10)
_cell_measurement_reflns_used    18763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.0590
_cell_measurement_theta_min      2.9720
_cell_volume                     1866.05(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -88.00 -62.00   0.50    0.20    --  -39.58 -69.00  56.00   52
  2  \w    -56.00 -31.00   0.50    0.20    --  -39.58  69.00-171.00   50
  3  \w    -11.00  20.00   0.50    0.20    --  -39.58  69.00-171.00   62
  4  \w     76.00 157.00   0.50    0.30    --   94.79  69.00-171.00  162
  5  \w     92.00 117.00   0.50    0.30    --   94.79 -69.00  56.00   50
  6  \w     39.00  65.00   0.50    0.30    --   94.79 -69.00  56.00   52
  7  \w    -58.00  24.00   0.50    0.20    --  -39.58  54.00   0.00  164
  8  \w    -15.00  25.00   0.50    0.20    --  -39.58  65.00  90.00   80
  9  \w    -58.00 -32.00   0.50    0.20    --  -39.58 -32.00  30.00   52
 10  \w    -57.00 -15.00   0.50    0.20    --  -39.58 138.00-150.00   84
 11  \w    -55.00 -29.00   0.50    0.20    --  -39.58 -69.00  56.00   52
 12  \w    -60.00 -20.00   0.50    0.20    --  -39.58  65.00  90.00   80
 13  \w    -93.00 -65.00   0.50    0.20    --  -39.58 138.00-150.00   56
 14  \w    -66.00 -14.00   0.50    0.20    --  -39.58 138.00 -30.00  104
 15  \w    -94.00 -69.00   0.50    0.20    --  -39.58 138.00 -30.00   50
 16  \w     24.00  60.00   0.50    0.20    --   39.58-138.00-150.00   72
 17  \w     69.00  98.00   0.50    0.20    --   39.58  43.00   0.00   58
 18  \w     31.00  57.00   0.50    0.20    --   39.58  54.00-120.00   52
 19  \w     65.00  93.00   0.50    0.20    --   39.58-138.00-150.00   56
 20  \w     31.00  60.00   0.50    0.20    --   39.58  43.00   0.00   58
 21  \w     30.00  62.00   0.50    0.20    --   39.58  32.00-180.00   64
 22  \w     63.00 102.00   0.50    0.20    --   39.58  69.00-171.00   78
 23  \w     69.00 100.00   0.50    0.20    --   39.58  54.00 120.00   62
 24  \w     26.00  51.00   0.50    0.20    --   39.58 -32.00 120.00   50
 25  \w     67.00 101.00   0.50    0.20    --   39.58  32.00-180.00   68
 26  \w     22.00  57.00   0.50    0.20    --   39.58  54.00 120.00   70
 27  \w     19.00  97.00   0.50    0.20    --   39.58  65.00 -90.00  156
 28  \w     21.00  46.00   0.50    0.20    --   39.58  69.00-171.00   50
 29  \w     34.00  59.00   0.50    0.20    --   39.58 -69.00  56.00   50
 30  \w     60.00 100.00   0.50    0.20    --   39.58  54.00-120.00   80
 31  \w     35.00  61.00   0.50    0.20    --   39.58  43.00 150.00   52
 32  \w     45.00 106.00   0.50    0.30    --   94.79 -42.00   0.00  122
 33  \w     46.00 115.00   0.50    0.30    --   94.79 -59.00-120.00  138
 34  \w     95.00 138.00   0.50    0.30    --   94.79  96.00 -90.00   86
 35  \w    112.00 149.00   0.50    0.30    --   94.79  68.00   0.00   74
 36  \w     38.00 105.00   0.50    0.30    --   94.79 -33.00-120.00  134
 37  \w     74.00  99.00   0.50    0.30    --   94.79-117.00 -60.00   50
 38  \w     63.00 111.00   0.50    0.30    --   94.79 -68.00  30.00   96
 39  \w    107.00 155.00   0.50    0.30    --   94.79  77.00 -60.00   96
 40  \w     49.00 116.00   0.50    0.30    --   94.79-145.00 -90.00  134
 41  \w     31.00 107.00   0.50    0.30    --   94.79-117.00 -90.00  152
 42  \w     88.00 150.00   0.50    0.30    --   94.79  77.00 120.00  124
 43  \w     74.00 109.00   0.50    0.30    --   94.79-117.00 150.00   70
 44  \w    119.00 151.00   0.50    0.30    --   94.79  77.00  30.00   64
 45  \w     36.00  61.00   0.50    0.30    --   94.79-117.00 150.00   50
 46  \w     29.00 107.00   0.50    0.30    --   94.79-117.00  60.00  156
 47  \w     97.00 132.00   0.50    0.30    --   94.79  33.00 120.00   70
 48  \w    101.00 126.00   0.50    0.30    --   94.79-145.00  60.00   50
 49  \w     57.00  89.00   0.50    0.30    --   94.79-145.00  60.00   64
 50  \w     83.00 144.00   0.50    0.30    --   94.79  77.00-150.00  122
 51  \w     80.00 141.00   0.50    0.30    --   94.79  59.00-180.00  122
 52  \w     24.00  96.00   0.50    0.30    --   94.79 -96.00  60.00  144
 53  \w     90.00 154.00   0.50    0.30    --   94.79  77.00  60.00  128
 54  \w    117.00 156.00   0.50    0.30    --   94.79  25.00 -90.00   78
 55  \w     42.00 108.00   0.50    0.30    --   94.79-145.00-120.00  132
 56  \w     27.00 119.00   0.50    0.30    --   94.79 -87.00 -90.00  184
 57  \w     76.00 157.00   0.50    0.30    --   94.79  59.00 150.00  162
 58  \w    -23.00   2.00   0.50    0.20    --  -39.58  69.00-171.00   50
 59  \w    -42.00 -17.00   0.50    0.20    --    4.00 119.00 173.24   50
 60  \w    -42.00 -17.00   0.50    0.20    --   20.00 145.00 163.31   50
 61  \w    -13.00  12.00   0.50    0.20    --   24.00 104.00 -55.60   50
 62  \w     -8.00  17.00   0.50    0.20    --   24.00  95.00  46.43   50
 63  \w     -8.00  17.00   0.50    0.20    --   24.00  96.00 -93.64   50
 64  \w      3.00  28.00   0.50    0.20    --   32.00  87.00 120.21   50
 65  \w      3.00  28.00   0.50    0.20    --   32.00  88.00 173.61   50
 66  \w      2.00  27.00   0.50    0.20    --   32.00  90.00 -50.05   50
 67  \w      2.00  27.00   0.50    0.20    --   32.00  89.00  19.96   50
 68  \w      2.00  27.00   0.50    0.20    --   32.00  90.00-159.85   50
 69  \w    -58.00 -33.00   0.50    0.20    --  -39.58  54.00 -60.00   50
 70  \w     13.00  38.00   0.50    0.20    --   39.58  81.00 -37.46   50
 71  \w     13.00  38.00   0.50    0.20    --   39.58  82.00  97.51   50
 72  \w     14.00  39.00   0.50    0.20    --   40.00  78.00-124.56   50
 73  \w     14.00  39.00   0.50    0.20    --   40.00  80.00-179.06   50
 74  \w     14.00  39.00   0.50    0.20    --   40.00  80.00 -46.16   50
 75  \w     14.00  42.00   0.50    0.20    --   40.00  81.00 -98.99   56
 76  \w     13.00  38.00   0.50    0.20    --   40.00  81.00  15.34   50
 77  \w     13.00  38.00   0.50    0.20    --   40.00  82.00  56.94   50
 78  \w     14.00  39.00   0.50    0.20    --   40.00  80.00 149.31   50
 79  \w     22.00  48.00   0.50    0.20    --   44.00  71.00 127.60   52
 80  \w     26.00  52.00   0.50    0.20    --   48.00  68.00  17.87   52
 81  \w     25.00  51.00   0.50    0.20    --   48.00  69.00  66.97   52
 82  \w     33.00  59.00   0.50    0.20    --   52.00  69.00 175.56   52
 83  \w     92.00 117.00   0.50    0.20    --   52.00  69.00 175.56   50
 84  \w     29.00  55.00   0.50    0.20    --   52.00  69.00 -86.06   52
 85  \w     91.00 117.00   0.50    0.20    --   52.00  69.00 -86.06   52
 86  \w     38.00  64.00   0.50    0.20    --   56.00  63.00 -12.60   52
 87  \w     37.00  62.00   0.50    0.20    --   60.00  71.00-160.11   50
 88  \w     86.00 124.00   0.50    0.20    --   60.00  70.00  30.95   76
 89  \w     37.00  75.00   0.50    0.20    --   60.00  70.00  30.95   76
 90  \w     37.00  63.00   0.50    0.20    --   60.00  70.00 -42.31   52
 91  \w     42.00  68.00   0.50    0.20    --   60.00  57.00 -93.89   52
 92  \w     37.00  62.00   0.50    0.20    --   60.00  69.00 146.14   50
 93  \w     50.00  97.00   0.50    0.20    --   64.00  71.00  84.12   94
 94  \w    104.00 129.00   0.50    0.20    --   64.00  66.00 -65.10   50
 95  \w     42.00  68.00   0.50    0.20    --   64.00  66.00 -65.10   52
 96  \w     41.00  66.00   0.50    0.20    --   64.00  70.00  65.40   50
 97  \w     46.00  83.00   0.50    0.30    --   68.00  64.00   4.27   74
 98  \w     50.00  76.00   0.50    0.30    --   72.00  65.00 -94.09   52
 99  \w     49.00  98.00   0.50    0.30    --   72.00  68.00-142.20   98
100  \w     50.00  76.00   0.50    0.30    --   72.00  67.00 -13.96   52
101  \w     59.00 131.00   0.50    0.30    --   72.00  54.00 -45.25  144
102  \w     49.00  75.00   0.50    0.30    --   72.00  68.00  74.96   52
103  \w     50.00  75.00   0.50    0.30    --   72.00  64.00 170.58   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1497044000
_diffrn_orient_matrix_UB_12      0.0393249000
_diffrn_orient_matrix_UB_13      -0.0445882000
_diffrn_orient_matrix_UB_21      0.0636226000
_diffrn_orient_matrix_UB_22      0.0991768000
_diffrn_orient_matrix_UB_23      0.0692066000
_diffrn_orient_matrix_UB_31      0.0921617000
_diffrn_orient_matrix_UB_32      0.0231687000
_diffrn_orient_matrix_UB_33      -0.0649412000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25125
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         3.008
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexafluorobenzene'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0348P)^2^+0.6366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6407
_reflns_number_total             6764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00651d2.cif
_cod_data_source_block           svb-548
_cod_database_code               7712882
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35 H33 Cl4 O2 N Pt '
_shelx_estimated_absorpt_t_max   0.435
_shelx_estimated_absorpt_t_min   0.368
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B)
1.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C1(H1), C24(H24), C2(H2), C26(H26), C3(H3), C4(H4), C30(H30),
 C9(H9), C11(H11), C10(H10), C18(H18), C19(H19), C20(H20)
1.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C)
1.d :
 C34(H34)
;
_shelx_res_checksum              97268
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.854