Semi-bridging σ-silyls as Z-type ligands.
Frogley, Benjamin J.; Hill, Anthony F.; Sharma, Manab; Sinha, Arup; Ward, Jas S.; Chemical communications (Cambridge, England) 56 (2020) 3532–3535; doi:10.1039/c9cc07763d

data_7126333
_publ_section_title
;
 Semi-bridging \s-silyls as Z-type ligands.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3532
_journal_page_last               3535
_journal_paper_doi               10.1039/c9cc07763d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C76 H66 N4 P4 Pd2 Si2, 2(C6 H6)'
_chemical_formula_sum            'C88 H78 N4 P4 Pd2 Si2'
_chemical_formula_weight         1584.40
_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
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-15 deposited with the CCDC.	2020-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.727(2)
_cell_angle_beta                 103.685(2)
_cell_angle_gamma                109.549(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5450(3)
_cell_length_b                   17.6245(6)
_cell_length_c                   17.7005(4)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1770
_cell_measurement_theta_min      3.6100
_cell_volume                     3724.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega  -25.00   55.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -38.0000  -60.0000 80

  2 omega   23.00   81.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000 -180.0000 58

  3 omega   24.00   88.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000  -30.0000 64

  4 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -45.0000    0.0000 58

  5 omega   54.00   88.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -45.0000  -90.0000 34

  6 omega   57.00  135.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -77.0000 -180.0000 78

  7 omega   91.00  172.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577   45.0000  -90.0000 81

  8 omega   43.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -45.0000   90.0000 55

  9 omega   47.00  107.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -95.0000   30.0000 60

 10 omega   40.00  106.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -95.0000  -60.0000 66

 11 omega   39.00   90.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -30.0000  -60.0000 51

 12 omega   38.00   76.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -30.0000 -120.0000 38

 13 omega   46.00  168.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577    0.0000   60.0000 122

 14 omega   39.00  110.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -95.0000  120.0000 71

 15 omega   40.00   98.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      107.9577  -45.0000  150.0000 58

 16 omega    6.00   72.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000   90.0000 66

 17 omega  -31.00   52.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000 -180.0000 83

 18 omega  -30.00   97.00   1.0000    1.0100
omega____ theta____ kappa____ phi______ frames
    -       36.0254    0.0000 -180.0000 127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      -0.0136319000
_diffrn_orient_matrix_UB_12      0.0483517000
_diffrn_orient_matrix_UB_13      0.0752679000
_diffrn_orient_matrix_UB_21      -0.0365710000
_diffrn_orient_matrix_UB_22      -0.0807553000
_diffrn_orient_matrix_UB_23      0.0271291000
_diffrn_orient_matrix_UB_31      0.1210582000
_diffrn_orient_matrix_UB_32      0.0206523000
_diffrn_orient_matrix_UB_33      0.0475284000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21940
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.426
_diffrn_reflns_theta_min         2.669
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.1903
_exptl_crystal_size_mid          0.1403
_exptl_crystal_size_min          0.0611
_refine_diff_density_max         3.433
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         14147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+7.0042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12345
_reflns_number_total             14147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07763d2.cif
_cod_data_source_block           AS2-24_Pd2
_cod_original_cell_volume        3724.14(19)
_cod_database_code               7126333
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C316) = Uanis(C311) = Uanis(C312) = Uanis(C313) = Uanis(C314) =
Uanis(C315)
Uanis(C107) = Uanis(C108) = Uanis(C109) = Uanis(C110) = Uanis(C111) =
Uanis(C112)
3.a Secondary CH2 refined with riding coordinates:
 C113(H11A,H11B), C120(H12A,H12B), C213(H21A,H21B), C220(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C115(H115), C116(H116),
 C117(H117), C118(H118), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C202(H202),
 C203(H203), C204(H204), C205(H205), C206(H206), C208(H208), C209(H209),
 C210(H210), C211(H211), C212(H212), C215(H215), C216(H216), C217(H217),
 C218(H218), C222(H222), C223(H223), C224(H224), C225(H225), C226(H226),
 C228(H228), C229(H229), C230(H230), C231(H231), C232(H232), C234(H234),
 C235(H235), C236(H236), C237(H237), C238(H238), C316(H316), C315(H315),
 C311(H311), C312(H312), C313(H313), C314(H314), C301(H301), C302(H302),
 C303(H303), C304(H304), C305(H305), C306(H306)
3.c Fitted hexagon refined as free rotating group:
 C316(C315,C311,C312,C313,C314)
;
_ins_header
;
TITL ARUP_1_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  13.544988  17.624474  17.700482  99.7268 103.6852 109.5491
ZERR    2.00   0.000307   0.000617   0.000399   0.0024   0.0019   0.0026
LATT  1
SFAC C H N Si P Pt
UNIT 152.00 132.00 8.00 4.00 8.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'