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_7126331
_publ_section_title
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 Semi-bridging \s-silyls as Z-type ligands.
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_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 Pt2 Si2, 2(C6 H6)'
_chemical_formula_sum            'C88 H78 N4 P4 Pt2 Si2'
_chemical_formula_weight         1761.78
_chemical_name_common            AS197
_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
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2016-11-15 deposited with the CCDC.	2020-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                70.8530(10)
_cell_angle_beta                 79.0290(10)
_cell_angle_gamma                88.9370(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9341(2)
_cell_length_b                   15.4591(3)
_cell_length_c                   20.0358(3)
_cell_measurement_reflns_used    124302
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.546
_cell_volume                     3711.20(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0364781
_diffrn_orient_matrix_UB_12      0.0297106
_diffrn_orient_matrix_UB_13      -0.0409888
_diffrn_orient_matrix_UB_21      -0.0694505
_diffrn_orient_matrix_UB_22      -0.0256632
_diffrn_orient_matrix_UB_23      0.0318134
_diffrn_orient_matrix_UB_31      -0.0078814
_diffrn_orient_matrix_UB_32      0.0561961
_diffrn_orient_matrix_UB_33      0.0144772
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            84642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.641
_exptl_absorpt_coefficient_mu    3.934
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         16970
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0355P)^2^+6.4199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13109
_reflns_number_total             16970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07763d2.cif
_cod_data_source_block           AS1-93_Pt2
_cod_database_code               7126331
_shelxl_version_number           2014/6
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C316 \\sim C311 \\sim C312 \\sim C313 \\sim C314 \\sim C315: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C121) = Uanis(C122) = Uanis(C123) = Uanis(C124) = Uanis(C125) =
Uanis(C126)
3. Rigid body (RIGU) restrains
 C316, C311, C312, C313, C314, C315
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C303, C302, C301, C306, C305, C304
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C113(H11A,H11B), C120(H12A,H12B), C213(H21A,H21B), C220(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), 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), C201(H201),
 C202(H202), C203(H203), C204(H204), C205(H205), 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), C303(H303), C302(H302),
 C301(H301), C306(H306), C305(H305), C304(H304), C316(H316), C311(H311),
 C312(H312), C313(H313), C314(H314), C315(H315)
4.c Fitted hexagon refined as free rotating group:
 C303(C302,C301,C306,C305,C304), C316(C311,C312,C313,C314,C315)
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_olex2_submission_special_instructions 'No special instructions were received'