Synthesis, Structure and Reactivity of µ3-SnH Capped Trinuclear Nickel Cluster
Torquato, Nicole A.; Mrse, Anthony A.; Gembicky, Milan; Chan, Thomas; Brunner, Felix M.; Kubiak, Clifford P.; Bertrand, Quentin C.; Palasz, Joseph M.; Chemical Science  (2022) –; doi:10.1039/D2SC04042E

data_1567597
_publ_section_title
;
 Synthesis, Structure and Reactivity of &#x00B5;3-SnH Capped Trinuclear
 Nickel Cluster
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04042E
_journal_year                    2022
_chemical_formula_moiety         'C81 H78 Ni3 P6 Sn'
_chemical_formula_sum            'C81 H78 Ni3 P6 Sn'
_chemical_formula_weight         1532.07
_chemical_name_systematic        2-hexeneSnNi3(dppm)3H
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                91.234(2)
_cell_angle_beta                 101.720(2)
_cell_angle_gamma                107.029(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9779(3)
_cell_length_b                   13.7494(4)
_cell_length_c                   23.0279(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.425
_cell_measurement_theta_min      3.374
_cell_volume                     3537.25(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62692
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.953
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             0.9
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.286
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.7792.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_preparation       '1 eq. 1-hexyne was added to HSnNi3(dppm)3H'
_exptl_crystal_recrystallization_method 'Et2O/C5 layering'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.719
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0082P)^2^+18.2823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10140
_reflns_number_total             12796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04042e2.cif
_cod_data_source_block           243_a
_cod_database_code               1567597
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.177
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All Ni(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 \\sim C6A-C5A \\sim C5A-C4 \\sim C5-C4
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C6A, C5A, C4, C3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C19(H19A,H19B),
 C44(H44A,H44B), C69(H69A,H69B), C5A(H5AA,H5AB)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
5.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              68549
_shelx_hkl_checksum              56485
_olex2_exptl_crystal_mounting_method 'paratone loop'
_olex2_submission_special_instructions 'No special instructions were received'