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_7132848
_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         'C43 H57 N4 Ni P2 Sc'
_chemical_formula_sum            'C43 H57 N4 Ni P2 Sc'
_chemical_formula_weight         795.53
_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
_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                101.880(3)
_cell_angle_beta                 96.172(3)
_cell_angle_gamma                90.996(3)
_cell_formula_units_Z            2
_cell_length_a                   11.122(2)
_cell_length_b                   11.696(2)
_cell_length_c                   16.447(3)
_cell_measurement_reflns_used    2172
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.336
_cell_measurement_theta_min      2.357
_cell_volume                     2079.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0836
_diffrn_reflns_av_unetI/netI     0.1554
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15514
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.273
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.6329.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     672
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3482
_reflns_number_total             7308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00547c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7132845--7132851.cif.'
_cod_original_cell_volume        2079.8(7)
_cod_database_code               7132848
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.899
_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 planarity
 C12, C8, C9, C11, C13, C10, C7, C14
 with sigma of 0.1
 C13, C11, C10, C8, C12, C9, C7, C14
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C8 \\sim C38A \\sim C13A \\sim C9 \\sim C9A \\sim C10 \\sim C26A \\sim C11
\\sim C42A \\sim C12 \\sim C11A \\sim C13 \\sim C24A \\sim C14 \\sim C28A \\sim
C24 \\sim C40A \\sim C25 \\sim C8A \\sim C26 \\sim C10A \\sim C27 \\sim C12A
\\sim C28 \\sim C14A \\sim C29 \\sim C25A \\sim C38 \\sim C27A \\sim C39 \\sim
C29A \\sim C40 \\sim C39A \\sim C41 \\sim C41A \\sim C42 \\sim C43A \\sim C43:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C24A)
\\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C40A)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{P1, C38A, C39A, C40A, C41A, C42A, C43A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1, C38, C39, C40, C41, C42, C43}
{P2, C24A, C25A, C26A, C27A, C28A, C29A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P2, C24, C25, C26, C27, C28, C29}
{C7, C8A, C9A, C10A, C11A, C12A, C13A, C14A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C7, C8, C9, C10, C11, C12, C13, C14}
5. Others
 Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(2)
 Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(2)
 Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41), C24(H24), C27(H27), C24A(H24A), C27A(H27A), C38A(H38A),
 C41A(H41A)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C30(H30A,H30B), C37(H37A,H37B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C12(H12), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C32(H32), C33(H33), C34(H34), C35(H35), C9A(H9A),
  C10A(H10A), C12A(H12A), C13A(H13A)
6.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F), C39A(H39D,
 H39E,H39F), C40A(H40D,H40E,H40F), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F)
;
_shelx_res_checksum              52861
_olex2_submission_special_instructions 'No special instructions were received'