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_7060254
_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         'C64 H108 Ni2 P4 Si4'
_chemical_formula_sum            'C64 H108 Ni2 P4 Si4'
_chemical_formula_weight         1231.12
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-09-12
_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                70.53(3)
_cell_angle_beta                 80.01(3)
_cell_angle_gamma                76.47(3)
_cell_formula_units_Z            2
_cell_length_a                   11.740(2)
_cell_length_b                   15.220(3)
_cell_length_c                   21.430(4)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2121
_cell_measurement_theta_min      2.1213
_cell_volume                     3490.9(13)
_computing_cell_refinement       'SAINT v6.02A (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.02A (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.1874
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23601
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.013
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.753
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5935
_reflns_number_total             12173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04079g2.cif
_cod_data_source_block           mono
_cod_original_cell_volume        3490.9(14)
_cod_original_formula_sum        'C64 H108 Ni2  P4 Si4'
_cod_database_code               7060254
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Si(H) groups
2.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2), Si3(H3), Si4(H4), C15(H15), C21(H21), C27(H27), C33(H33),
 C41(H41), C47(H47), C53(H53), C59(H59)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              53792
_shelx_fab_checksum              41330
_olex2_submission_special_instructions 'No special instructions were received'