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_7132850
_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         'C94 H118 N10 Ni2 O2 P4 Sc2, 4(C6 H6)'
_chemical_formula_sum            'C118 H142 N10 Ni2 O2 P4 Sc2'
_chemical_formula_weight         2063.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 109.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.918(6)
_cell_length_b                   11.542(2)
_cell_length_c                   36.001(7)
_cell_measurement_reflns_used    7850
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      23.662
_cell_measurement_theta_min      2.205
_cell_volume                     11330(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0718
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            48798
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         1.200
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0495 after correction.
The Ratio of minimum to maximum transmission is 0.6341.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         12844
_refine_ls_number_restraints     1761
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5597
_reflns_number_total             12844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00547c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7132845--7132851.cif.'
_cod_database_code               7132850
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.922
_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
 C59-C58 = C58-C57 = C57-C56 = C56-C55 = C55-C54 = C59-C54
 1.39 with sigma of 0.01
 C52-C51 = C53-C52 = C53-C48 = C49-C48 = C50-C49 = C51-C50
 1.39 with sigma of 0.01
 C53A-C52A = C53A-C48A = C49A-C48A = C50A-C49A = C51A-C50A = C52A-C51A
 1.39 with sigma of 0.01
 C54-C56 \\sim C55-C57 \\sim C56-C58 \\sim C57-C59 \\sim C58-C54 \\sim C59-C55
 with sigma of 0.02
 Ni1-P1A \\sim Ni1-P1
 with sigma of 0.02
 Sc1-O1A \\sim Sc1-O1
 with sigma of 0.02
 C35-C34 \\sim C35-C34A
 with sigma of 0.02
 Sc1-N2 \\sim Sc1-N2A
 with sigma of 0.02
 Sc1-N1 \\sim Sc1-N1A
 with sigma of 0.02
3. Restrained planarity
 C54, C55, C56, C57, C58, C59
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C49A \\sim C48A
\\sim C53A \\sim C50A \\sim C52A \\sim C51A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C54A \\sim C55A
\\sim C56A \\sim C57A \\sim C58A \\sim C59A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N1 \\sim N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C19 \\sim C20
\\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C29 \\sim N1A
\\sim N3A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C19A \\sim
C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim
C29A \\sim N2 \\sim C34 \\sim N2A \\sim C34A \\sim O1 \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17 \\sim C18 \\sim C27 \\sim C32 \\sim O1A \\sim C6A \\sim C7A \\sim
C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A
\\sim C16A \\sim C17A \\sim C18A \\sim C27A \\sim C32A \\sim P1 \\sim C28 \\sim
C31 \\sim P1A \\sim C31A \\sim C30 \\sim C33 \\sim C30A \\sim C33A \\sim Sc1
\\sim Ni1 \\sim C35: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
5. Same fragment restrains
{P1A, O1A, N1A, N2A, N3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A,
C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A,
C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A} sigma for
1-2: 0.02, 1-3: 0.04
as in
{P1, O1, N1, N2, N3, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13,
C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29,
C30, C31, C32, C33, C34}
{C48A, C49A, C50A, C51A, C52A, C53A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C48, C49, C50, C51, C52, C53}
{C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C54, C55, C56, C57, C58, C59}
6. Others
 Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=
 Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=1-FVAR(1)
 Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=
 Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=FVAR(1)
 Sof(P1A)=Sof(O1A)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=
 Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19C)=
 Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
 Sof(H31A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34C)=Sof(H34D)=1-FVAR(2)
 Sof(P1)=Sof(O1)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=
 Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=
 Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=FVAR(2)
 Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=
 Sof(H51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=1-FVAR(3)
 Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C42(H42), C45(H45), C28(H28), C31(H31), C28A(H28A), C31A(H31A)
7.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C19(H19A,H19B), C20(H20A,H20B), C27(H27A,H27B), C34(H34A,
 H34B), C19A(H19C,H19D), C20A(H20C,H20D), C27A(H27C,H27D), C34A(H34C,H34D)
7.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C2(H2), C3(H3), C4(H4), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C2A(H2A), C3A(H3A), C4A(H4A),
  C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C14A(H14A),
 C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C22A(H22A), C23A(H23A),
 C24A(H24A), C25A(H25A), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C54A(H54A), C55A(H55A), C56A(H56A), C57A(H57A), C58A(H58A), C59A(H59A),
 C48A(H48A), C49A(H49A), C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A)
7.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C32A(H32D,H32E,H32F),
 C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              16722
_olex2_submission_special_instructions 'No special instructions were received'