Atomically precise structures of Pt<sub>2</sub>(S-Adam)<sub>4</sub>(PPh<sub>3</sub>)<sub>2</sub> complexes and catalytic application in propane dehydrogenation.
Lin, Xinzhang; Zhang, Junying; Tang, Jie; Yang, Yang; Liu, Chao; Huang, Jiahui; Nanoscale 14 (2022) 2482–2489; doi:10.1039/d1nr07286b

data_1565931
_publ_section_title
;
 Atomically precise structures of
 Pt<sub>2</sub>(S-Adam)<sub>4</sub>(PPh<sub>3</sub>)<sub>2</sub> complexes
 and catalytic application in propane dehydrogenation.
;
_journal_issue                   6
_journal_name_full               Nanoscale
_journal_page_first              2482
_journal_page_last               2489
_journal_paper_doi               10.1039/d1nr07286b
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C76 H90 P2 Pt2 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C78 H94 Cl4 P2 Pt2 S4'
_chemical_formula_weight         1753.69
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2021-02-03 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.940(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7531(5)
_cell_length_b                   23.1655(12)
_cell_length_c                   13.3165(7)
_cell_measurement_reflns_used    8281
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5760
_cell_measurement_theta_min      4.0230
_cell_volume                     3606.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4070
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.850
_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      7.00  50.00   1.00   14.19    --   -9.27  57.00   0.00   43
  2  \w    -31.00   0.00   1.00   14.19    --   -9.27  57.00   0.00   31
  3  \w     -4.00  48.00   1.00   14.19    --    9.34 -99.00-180.00   52
  4  \w    -40.00  38.00   1.00   14.19    --    9.34 -19.00-150.00   78
  5  \w     22.00  48.00   1.00   14.19    --    9.34 -99.00  60.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0162147000
_diffrn_orient_matrix_UB_12      -0.0043159000
_diffrn_orient_matrix_UB_13      0.0523134000
_diffrn_orient_matrix_UB_21      0.0347578000
_diffrn_orient_matrix_UB_22      -0.0236157000
_diffrn_orient_matrix_UB_23      -0.0114801000
_diffrn_orient_matrix_UB_31      0.0469836000
_diffrn_orient_matrix_UB_32      0.0189692000
_diffrn_orient_matrix_UB_33      -0.0024098000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24624
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.815
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8797
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+1.3346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7056
_reflns_number_total             8797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr07286b2.cif
_cod_data_source_block           lxz-1-180427
_cod_depositor_comments
'Adding full bibliography for 1565931--1565933.cif.'
_cod_database_code               1565931
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H S P Pt Ag'
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.631
_reflns_odcompleteness_completeness 99.83
_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, All C(H,H,H,H) groups
2. Restrained distances
 Cl1-C39 \\sim Cl1A-C39
 with sigma of 0.02
3. Others
 Sof(H39C)=Sof(H39D)=Sof(Cl1A)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(Cl1)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C13(H13), C15(H15), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C39(H39A,H39B), C39(H39C,H39D)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              84727
_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 1.168
_oxdiff_exptl_absorpt_empirical_full_min 0.822