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_1567596
_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         'C77 H72 Br Ni3 P6 Sn, C4 H8 O'
_chemical_formula_sum            'C81 H80 Br Ni3 O P6 Sn'
_chemical_formula_weight         1630.00
_chemical_name_systematic        Br(CH3CH2)HSnNi3(dppm)3H
_chemical_properties_physical    Air-sensitive,Moisture-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             2022-05-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.583(2)
_cell_angle_beta                 102.885(2)
_cell_angle_gamma                112.374(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6920(6)
_cell_length_b                   13.0930(8)
_cell_length_c                   24.4579(14)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.75
_cell_volume                     3643.3(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1298
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89348
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.087
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_min         2.535
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.5619
_exptl_absorpt_correction_T_min  0.3681
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1648 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.6551.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1666
_exptl_crystal_preparation       '1 Eq. BrCH2CH3 was added to HSnNi3(dppm)3H'
_exptl_crystal_recrystallization_method
'The material was recrystallised from THF by solvent layering of pentane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         12914
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0346P)^2^+9.5360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8904
_reflns_number_total             12914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04042e2.cif
_cod_data_source_block           265d_a
_cod_database_code               1567596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. 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
2. Restrained distances
 Ni2-H \\sim Ni3-H \\sim Ni1-H
 with sigma of 0.01
3. Others
 Fixed Uiso: H(0.025)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C25(H25A,
 H25B), C50(H50A,H50B), C75(H75A,H75B), C77(H77A,H77B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), 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), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), 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), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
4.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C)
;
_shelx_res_checksum              23509
_shelx_hkl_checksum              57178
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'