Understanding the Solution and Solid-State Structures of Pd and Pt PSiP Pincer-Supported Hydrides.
Suh, Hee-Won; Balcells, David; Edwards, Alison J.; Guard, Louise M.; Hazari, Nilay; Mader, Elizabeth A.; Mercado, Brandon Q.; Repisky, Michal; Inorganic chemistry 54 (2015) 11411–11422; doi:10.1021/acs.inorgchem.5b02073

data_4344448
_publ_section_title
;
 Understanding the Solution and Solid-State Structures of Pd and Pt PSiP
 Pincer-Supported Hydrides.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11411
_journal_page_last               11422
_journal_paper_doi               10.1021/acs.inorgchem.5b02073
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '4(C37 H56 P2 Pt Si), 5(C5 H12)'
_chemical_formula_sum            'C173 H284 P8 Pt4 Si4'
_chemical_formula_weight         3504.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2013-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
END
;
_cell_angle_alpha                90
_cell_angle_beta                 99.690(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.5946(5)
_cell_length_b                   17.3883(3)
_cell_length_c                   33.970(2)
_cell_measurement_reflns_used    100729
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      2.6
_cell_volume                     17231.6(12)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      93
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 180.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 180.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 220.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 50.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 125.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 55.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 225.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 300.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 250.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 320.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 110.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 150.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 75.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 350.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 275.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 25.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 175.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 325.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: -48.0000 - 132.0000
         Image width: 2.0000
            Exp time: 2.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 165.0000
                 XTD: 42.6701
              2theta: 41.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 275.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 100.0000
                 XTD: 42.6701
              2theta: 89.0725
scan:
    Number of images: 90
               Slice: 0.0000 - 180.0000
         Image width: 2.0000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 200.0000
                 XTD: 42.6701
              2theta: 89.0725
;
_diffrn_measurement_device
;
AFC11 (Left): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn944+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.032600
_diffrn_orient_matrix_UB_12      -0.014105
_diffrn_orient_matrix_UB_13      -0.010319
_diffrn_orient_matrix_UB_21      -0.005037
_diffrn_orient_matrix_UB_22      -0.010166
_diffrn_orient_matrix_UB_23      0.027911
_diffrn_orient_matrix_UB_31      -0.009322
_diffrn_orient_matrix_UB_32      0.054819
_diffrn_orient_matrix_UB_33      0.002521
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            297570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.353
_diffrn_reflns_theta_min         2.639
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    7.249
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       Block
_exptl_crystal_F_000             7240
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         15754
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+60.4757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15097
_reflns_number_total             15754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02073_si_002.cif
_cod_data_source_block           '_(CyPSiP)PtH_Polymorph_2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4344446--4344451.cif.
;
_cod_original_cell_volume        17231.5(12)
_cod_database_code               4344448
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.713
_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. Restrained distances
 C82-C81 \\sim C81-C80
 with sigma of 0.02
 C78-C79 \\sim C77-C78 \\sim C76-C77 \\sim C75-C76
 with sigma of 0.02
 C79-C77 \\sim C77-C75
 with sigma of 0.02
 C87-C83 \\sim C83-C85
 with sigma of 0.02
 C78A-C76A \\sim C76-C78
 with sigma of 0.02
 C79A-C78A \\sim C78A-C77A \\sim C77A-C76A \\sim C76A-C75A \\sim C79-C78 \\sim
C78-C77 \\sim C77-C76 ~
 C76-C75 \\sim C85-C84 \\sim C84-C83 \\sim C86-C83 \\sim C87-C86
 with sigma of 0.02
 C79A-C75A \\sim C79-C75
 with sigma of 0.02
 C75A-C77A \\sim C77A-C79A
 with sigma of 0.02
3. Rigid bond restraints
 C80, C81, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C77, C79, C78, C76, C79A, C77A, C75A, C76A, C78A, C75, C85, C84, C83, C86, C87
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C82 \\sim C81 \\sim C80: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C77 \\sim C76 \\sim C75 \\sim C79A \\sim C77A \\sim C75A \\sim C76A \\sim C78A
\\sim C79 \\sim C78 \\sim C85 \\sim C84 \\sim C83 \\sim C86 \\sim C87: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C79A) = Uanis(C78A)
5. Others
 Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C77A)=Sof(H77C)=Sof(H77D)=
 Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76A)=Sof(H76C)=Sof(H76D)=
 Sof(C78A)=Sof(H78C)=Sof(H78D)=1-FVAR(1)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C78)=
 Sof(H78A)=Sof(H78B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C75)=Sof(H75A)=Sof(H75B)=
 Sof(H75C)=FVAR(1)
 Fixed Sof: H(0.5) HA(0.5)
6.a Ternary CH refined with riding coordinates:
 C44(H44), C38(H38), C26(H26), C1(H1A), C7(H7), C69(H69), C63(H63), C32(H32)
6.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C31(H31A,H31B), C12(H12A,H12B), C39(H39A,H39B), C8(H8A,H8B),
 C41(H41A,H41B), C47(H47A,H47B), C2(H2A,H2B), C11(H11A,H11B), C3(H3A,H3B),
 C5(H5A,H5B), C6(H6A,H6B), C27(H27A,H27B), C9(H9A,H9B), C46(H46A,H46B),
 C10(H10A,H10B), C43(H43A,H43B), C49(H49A,H49B), C70(H70A,H70B), C74(H74A,H74B),
  C40(H40A,H40B), C33(H33A,H33B), C67(H67A,H67B), C30(H30A,H30B), C34(H34A,
 H34B), C4(H4A,H4B), C48(H48A,H48B), C37(H37A,H37B), C68(H68A,H68B), C28(H28A,
 H28B), C42(H42A,H42B), C64(H64A,H64B), C66(H66A,H66B), C71(H71A,H71B),
 C65(H65A,H65B), C72(H72A,H72B), C35(H35A,H35B), C29(H29A,H29B), C73(H73A,H73B),
  C36(H36A,H36B), C77(H77A,H77B), C78(H78A,H78B), C76(H76A,H76B), C77A(H77C,
 H77D), C76A(H76C,H76D), C78A(H78C,H78D), C80(H,HA), C81(H81A,H81B), C83(H83A,
 H83B), C84(H84A,H84B), C86(H86A,H86B)
6.c Me refined with riding coordinates:
 C79(H79A,H79B,H79C), C75(H75A,H75B,H75C), C79A(H79D,H79E,H79F), C75A(H75D,
 H75E,H75F), C82(H82A,H82B,H82C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C)
6.d Aromatic/amide H refined with riding coordinates:
 C54(H54), C51(H51), C23(H23), C17(H17), C21(H21), C22(H22), C24(H24),
 C53(H53), C60(H60), C14(H14), C52(H52), C58(H58), C16(H16), C15(H15), C59(H59),
  C61(H61)
6.e Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              36772
_shelx_hkl_checksum              41558