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_1567595
_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         'C75 H67 Ni3 P6 Sn, C4 H10 O1'
_chemical_formula_sum            'C79 H77 Ni3 O P6 Sn'
_chemical_formula_weight         1523.04
_chemical_name_systematic        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             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-09 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.2340(10)
_cell_angle_beta                 74.0990(10)
_cell_angle_gamma                85.0760(10)
_cell_formula_units_Z            2
_cell_length_a                   15.7957(16)
_cell_length_b                   15.8530(16)
_cell_length_c                   15.9408(16)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.44
_cell_volume                     3824.7(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_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       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0872
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35268
_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         25.687
_diffrn_reflns_theta_min         1.289
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.2522
_exptl_absorpt_correction_T_min  0.2106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0873 after correction.
The Ratio of minimum to maximum transmission is 0.8351.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1566
_exptl_crystal_preparation
'4 eq. of NaB(Et)3H was added to Cl3SnNi3(dppm)3Cl'
_exptl_crystal_recrystallization_method
'Vapor diffusion of Et2O into a THF solution of HSnNi3(dppm)3H'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         14525
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.0475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11964
_reflns_number_total             14525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04042e2.cif
_cod_data_source_block           112_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1567595
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.712
_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
 C38-C33 \\sim C38A-C33A \\sim C38-C37 \\sim C38A-C37A \\sim C37-C36 \\sim
C37A-C36A \\sim C36-C35 ~
 C36A-C35A \\sim C35-C34 \\sim C35A-C34A \\sim C34-C33 \\sim C34A-C33A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C33A) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1S) = Uanis(C1T)
4. Rigid body (RIGU) restrains
 P3, C33A, C34A, C35A, C36A, C37A, C38A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 P3, C33, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1T, C2T, O1T, C3T, C4T
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1S, C2S, O1S, C3S, C4S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{O1S, C1S, C2S, C3S, C4S} sigma for 1-2: 0.005, 1-3: 0.01
as in
{O1T, C1T, C2T, C3T, C4T}
6. Others
 Sof(C33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=1-FVAR(1)
 Sof(C33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=
 Sof(H37)=Sof(C38)=Sof(H38)=FVAR(1)
 Sof(O1T)=Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(H1TC)=Sof(C2T)=Sof(H2TA)=Sof(H2TB)=
 Sof(C3T)=Sof(H3TA)=Sof(H3TB)=Sof(C4T)=Sof(H4TA)=Sof(H4TB)=Sof(H4TC)=1-FVAR(2)
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=
 Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=FVAR(2)
 Fixed Uiso: H(0.0235)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C25(H25A,H25B), C51(H51A,H51B), C2S(H2SA,H2SB), C3S(H3SA,H3SB),
 C2T(H2TA,H2TB), C3T(H3TA,H3TB)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C34A(H34A), C35(H35), C35A(H35A), C36(H36), C36A(H36A),
 C37(H37), C37A(H37A), C38(H38), C38A(H38A), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61),
 C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C71(H71),
  C72(H72), C73(H73), C74(H74), C75(H75)
7.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC), C1T(H1TA,H1TB,H1TC), C4T(H4TA,H4TB,
 H4TC)
;
_shelx_res_checksum              81562
_shelx_hkl_checksum              7470
_shelx_fab_checksum              46617
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'