A scandium metalloligand supported Ni(0) complex with a heterobimetallocycle: versatile reactivity with unsaturated bonds.
Ma, Lei; Pan, Xiaowei; Hong, Dongjing; Fang, Huayi; Cui, Peng; Chemical communications (Cambridge, England) 60 (2024) 4222–4225; doi:10.1039/d4cc00547c

data_7132845
_publ_section_title
;
 A scandium metalloligand supported Ni(0) complex with a
 heterobimetallocycle: versatile reactivity with unsaturated bonds.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4222
_journal_page_last               4225
_journal_paper_doi               10.1039/d4cc00547c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H61 N4 P2 Sc Si'
_chemical_formula_sum            'C38 H61 N4 P2 Sc Si'
_chemical_formula_weight         708.89
_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
_audit_creation_date             2023-12-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.496(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5452(10)
_cell_length_b                   15.3097(10)
_cell_length_c                   17.8477(12)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.326
_cell_measurement_theta_min      2.659
_cell_volume                     4211.3(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II 293K'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            93215
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.7696.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9649
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0703P)^2^+4.8080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5974
_reflns_number_total             9649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00547c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7132845--7132851.cif.'
_cod_database_code               7132845
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.952
_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
 C31A-C29A = C31-C29 = C30-C29 = C30A-C29A = C34-C32 = C33-C32 = C33A-C32A =
 C34A-C32A
 1.54 with sigma of 0.01
 C30A-C31A = C31-C30 = C33-C34 = C33A-C34A
 2.515 with sigma of 0.02
 N4-C28 \\sim N4-C28A
 with sigma of 0.02
 C32-C29 \\sim C29A-C32A
 with sigma of 0.02
 P2A-C28A \\sim P2-C28
 with sigma of 0.02
 P2A-C32A \\sim P2-C32
 with sigma of 0.02
 P2-C29 \\sim P2A-C29A
 with sigma of 0.02
 Sc1-N1 \\sim Sc1-N1A
 with sigma of 0.02
 N2-C6A \\sim N2-C6
 with sigma of 0.02
 C6A-C5A \\sim C6-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim C32 \\sim C29 \\sim C30 \\sim C34 \\sim C33 \\sim C31 \\sim P2A \\sim
C32A \\sim C29A \\sim C30A \\sim C34A \\sim C33A \\sim C31A \\sim C28 \\sim
C28A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
N1 \\sim C6 \\sim C5 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C2A \\sim C4A
\\sim C5A \\sim C1A \\sim N1A \\sim C6A \\sim C3A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 P2, C32, C29, C30, C34, C33, C31, P2A, C32A, C29A, C30A, C34A, C33A, C31A, N4,
  C28, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N1, C6, C5, C1, C2, C3, C4, C2A, C4A, C5A, C1A, N1A, C6A, C3A, Sc1, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Same fragment restrains
{N1A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{N1, C1, C2, C3, C4, C5, C6}
6. Others
 Sof(P2A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C32A)=Sof(H32A)=Sof(C29A)=
 Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C34A)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(P2)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C32)=Sof(H32)=Sof(C29)=Sof(H29)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 FVAR(1)
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(2)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C18(H18), C15(H15), C32(H32), C29(H29), C32A(H32A), C29A(H29A)
7.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C7(H7A,H7B), C21(H21A,H21B), C28(H28A,H28B),
 C35(H35A,H35B), C28A(H28C,H28D), C6A(H6AA,H6AB)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C26(H26), C9(H9), C23(H23), C12(H12),
 C25(H25), C24(H24), C10(H10), C11(H11), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A)
7.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C38(H38A,H38B,
 H38C), C36(H36A,H36B,H36C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C34(H34A,
 H34B,H34C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C),
 C30A(H30D,H30E,H30F), C34A(H34D,H34E,H34F), C33A(H33D,H33E,H33F), C31A(H31D,
 H31E,H31F)
;
_shelx_res_checksum              35677
_olex2_submission_special_instructions 'No special instructions were received'