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_1567598
_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 H71 I Ni3 P6 Sn, C6 H6'
_chemical_formula_sum            'C83 H77 I Ni3 P6 Sn'
_chemical_formula_weight         1681.98
_chemical_name_systematic        Ch3Ch2SnNi3(dppm)3I
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-27
_audit_creation_method
;
Olex2 1.5-alpha
(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                90
_cell_angle_beta                 103.455(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0909(10)
_cell_length_b                   22.5824(12)
_cell_length_c                   20.2582(12)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.377
_cell_measurement_theta_min      2.255
_cell_volume                     7159.2(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.5-alpha (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0580
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            118231
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.023
_diffrn_reflns_theta_min         2.172
_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    1.733
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.4115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1205 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8393.
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    1.561
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3408
_exptl_crystal_preparation       'iodoethane was added to HSnNi3(dppm)3H'
_exptl_crystal_recrystallization_method 'd-benzene/c5 layering'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0123P)^2^+11.1866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11715
_reflns_number_total             14079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04042e2.cif
_cod_data_source_block           250_a
_cod_database_code               1567598
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.582
_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. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(Sn1A)
Uanis(Sn1) = Uanis(I1A)
3. Others
 Sof(I1A)=Sof(Sn1A)=1-FVAR(1)
 Sof(I1)=Sof(Sn1)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C15(H15A,H15B), C40(H40A,H40B), C65(H65A,H65B)
4.b Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4(H4), C4S(H4S), C5(H5), C5S(H5S), C6(H6),
 C6S(H6S), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62),
  C63(H63), C64(H64), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
 C73(H73), C74(H74), C75(H75), C76(H76), C77(H77)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              73401
_shelx_hkl_checksum              10154
_olex2_exptl_crystal_mounting_method 'paratone loop'
_olex2_submission_special_instructions 'No special instructions were received'