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_7132846
_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         'C68 H98 N10 Ni2 P4 Sc2, C5 H12'
_chemical_formula_sum            'C73 H110 N10 Ni2 P4 Sc2'
_chemical_formula_weight         1458.92
_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                65.861(6)
_cell_angle_beta                 73.439(6)
_cell_angle_gamma                76.945(6)
_cell_formula_units_Z            1
_cell_length_a                   12.490(6)
_cell_length_b                   12.540(6)
_cell_length_c                   13.517(6)
_cell_measurement_reflns_used    5689
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.049
_cell_measurement_theta_min      2.321
_cell_volume                     1837.3(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.961
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16504
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.736
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1025 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.6257.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8325
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0515P)^2^+0.1479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5868
_reflns_number_total             8325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00547c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7132845--7132851.cif.'
_cod_original_cell_volume        1837.2(15)
_cod_database_code               7132846
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.887
_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with polybutenes oil (CAS: 9003-29-6) on a glass slide. A suitable single crystal coated with polybutenes oil as less as possible was sealed in capillary tube filled with argon. The capillary tube with single crystal was mounted on copper pin with solid paraffin.'
_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
 C36-C35 = C37-C36 = C38-C37 = C39-C38
 1.54 with sigma of 0.01
 C35-C37 = C36-C38 = C37-C39
 2.515 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C36 \\sim C35 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C36, C35, C37, C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) C36(0.5) H36A(0.5) H36B(0.5) C38(0.5) H38A(0.5) H38B(0.5) C39(0.5)
 H39A(0.5) H39B(0.5) H39C(0.5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C29(H29), C32(H32)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B),
 C37(H37A,H37B), C36(H36A,H36B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C23(H23),
 C24(H24), C25(H25), C26(H26)
6.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              88584
_olex2_submission_special_instructions 'No special instructions were received'