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_7132849
_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         'C42 H56 N5 Ni P2 Sc, 1.5(C4 H8 O)'
_chemical_formula_sum            'C48 H68 N5 Ni O1.5 P2 Sc'
_chemical_formula_weight         904.68
_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   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                77.96(3)
_cell_angle_beta                 79.02(4)
_cell_angle_gamma                81.49(5)
_cell_formula_units_Z            2
_cell_length_a                   10.142(14)
_cell_length_b                   10.213(12)
_cell_length_c                   23.78(3)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.140
_cell_measurement_theta_min      2.642
_cell_volume                     2350(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1307
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            94236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.6898.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10783
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0572P)^2^+5.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7118
_reflns_number_total             10783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00547c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7132845--7132851.cif.'
_cod_original_cell_volume        2349(5)
_cod_original_formula_sum        'C48 H68 N5 Ni O1.50 P2 Sc'
_cod_database_code               7132849
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.920
_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
 O2-C50 = O2-C47 = O2A-C50A = O2A-C47A = O1-C43 = O1-C46
 1.43 with sigma of 0.01
 C44-C43 = C45-C44 = C46-C45 = C48A-C47A = C49-C48 = C50-C49 = C50A-C49A =
 C49A-C48A = C48-C47
 1.54 with sigma of 0.01
 O1-C44 = O1-C45 = O2-C48 = O2-C49 = O2A-C48A = O2A-C49A
 2.426 with sigma of 0.02
 C43-C46 = C47-C50 = C50A-C47A
 2.336 with sigma of 0.02
 C47-C49 = C48-C50 = C50A-C48A = C47A-C49A = C43-C45 = C46-C44
 2.515 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C43 \\sim C46 \\sim C44 \\sim C45 \\sim O2 \\sim C50 \\sim C47 \\sim
C49 \\sim C48 \\sim C47A \\sim O2A \\sim C50A \\sim C49A \\sim C48A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C44) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C47) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(O2A) \\sim Ueq,
Uanis(C50A) \\sim Ueq, Uanis(C49A) \\sim Ueq, Uanis(C48A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O2A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C47A)=Sof(H47C)=Sof(H47D)=
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(O2)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(C47)=Sof(H47A)=Sof(H47B)=FVAR(1)
 Fixed Sof: O1(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26), C37(H37), C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C22(H22A,H22B), C29(H29A,H29B), C36(H36A,
 H36B), C50(H50A,H50B), C49(H49A,H49B), C48(H48A,H48B), C47(H47A,H47B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C50A(H50C,
 H50D), C47A(H47C,H47D), C49A(H49C,H49D), C48A(H48C,H48D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C11(H11), C12(H12), C17(H17),
 C18(H18), C19(H19), C20(H20), C31(H31), C32(H32), C33(H33), C34(H34)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              36488
_olex2_submission_special_instructions 'No special instructions were received'