Trapping of two mononuclear silyl platinum(ii)/palladium(ii) complexes and a unique dinuclear bis(μ2-disilene)(silyl)nickel(ii) complex
Song, Hao; Zhang, Sen-Yu; Gu, Peng-Fei; Wu, Hua-Yu; Wang, Zi-Kun; Wang, Shi; Wang, Zheng; Gu, Yu-Yang; Li, Yong-Hua; New Journal of Chemistry 44 (2020) 20351–20357; doi:10.1039/D0NJ04079G

data_7060253
_publ_section_title
;
 Trapping of two mononuclear silyl platinum(ii)/palladium(ii) complexes
 and a unique dinuclear bis(\m2-disilene)(silyl)nickel(ii) complex
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20351
_journal_page_last               20357
_journal_paper_doi               10.1039/D0NJ04079G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C18 H36 O2 P2 Pt Si2'
_chemical_formula_sum            'C18 H36 O2 P2 Pt Si2'
_chemical_formula_weight         597.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-16 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6370(17)
_cell_length_b                   15.795(3)
_cell_length_c                   18.196(4)
_cell_measurement_reflns_used    4623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1984
_cell_measurement_theta_min      2.2905
_cell_volume                     2457.3(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20147
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.002
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_min         1.130
_exptl_absorpt_coefficient_mu    5.947
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         5.489
_refine_diff_density_min         -2.868
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.1075
_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^)+(0.0126P)^2^+372.5082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4187
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04079g2.cif
_cod_data_source_block           12q
_cod_database_code               7060253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.431
_shelx_estimated_absorpt_t_min   0.398
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8679(13)
 0.1321(13)
2. 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
3. Rigid bond restraints
 P2, C17, Si1, C8, Pt1, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(P2) \\sim Ueq, Uanis(Si2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              2669
_olex2_submission_special_instructions 'No special instructions were received'