Synthesis and characterization of heterotrimetallic Mg-Ni-Mg complexes with amidinato ligands.
Zhang, Rongping; Cai, Yanping; Xu, Xin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3437–3443; doi:10.1039/d4dt03495c

data_1573699
_publ_section_title
;
 Synthesis and characterization of heterotrimetallic Mg-Ni-Mg complexes
 with amidinato ligands.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3437
_journal_page_last               3443
_journal_paper_doi               10.1039/d4dt03495c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C96 H116 Mg2 N4 Ni P2, 4(C6 H6)'
_chemical_formula_sum            'C120 H140 Mg2 N4 Ni P2'
_chemical_formula_weight         1807.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-06 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.001(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2558(11)
_cell_length_b                   15.2714(9)
_cell_length_c                   18.9886(12)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      60.599
_cell_measurement_theta_min      3.324
_cell_volume                     5136.6(5)
_computing_cell_refinement       'SAINT V8.40B (2016)'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_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            113318
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.965
_diffrn_reflns_theta_min         3.635
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1367 before and 0.0867 after correction.
The Ratio of minimum to maximum transmission is 0.7795.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         10130
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+1.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8774
_reflns_number_total             10130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03495c2.cif
_cod_data_source_block           ga20240829xa_0ma_a
_cod_depositor_comments
'Adding full bibliography for 1573698--1573702.cif.'
_cod_database_code               1573699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Restrained distances
 C60-C59 = C63-C62 = C62-C61
 1.37 with sigma of 0.02
 C60-C61
 1.38 with sigma of 0.02
 C59-C58 = C58-C63
 1.36 with sigma of 0.02
 C53-C54 = C56-C57 = C57-C52
 1.37 with sigma of 0.02
 C53-C52
 1.38 with sigma of 0.02
 C54-C55 = C55-C56
 1.36 with sigma of 0.02
 C60-C58 = C58-C62 = C63-C61
 2.37 with sigma of 0.04
 C60-C62
 2.38 with sigma of 0.04
 C59-C63
 2.36 with sigma of 0.04
 C53-C55 = C55-C57 = C56-C52
 2.37 with sigma of 0.04
 C53-C57
 2.38 with sigma of 0.04
 C54-C56
 2.36 with sigma of 0.04
 C60-C59 \\sim C59-C58 \\sim C58-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60
 with sigma of 0.02
 C60-C62 \\sim C60-C58 \\sim C62-C58 \\sim C63-C59 \\sim C63-C61 \\sim C61-C59
 with sigma of 0.04
 C53-C54 \\sim C54-C55 \\sim C55-C56 \\sim C56-C57 \\sim C57-C52 \\sim C52-C53
 with sigma of 0.02
 C53-C57 \\sim C53-C55 \\sim C57-C55 \\sim C56-C54 \\sim C56-C52 \\sim C52-C54
 with sigma of 0.04
2. Restrained planarity
 C60, C59, C58, C63, C62, C61
 with sigma of 0.1
 C53, C54, C55, C56, C57, C52
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C60 \\sim C59 \\sim C58 \\sim C63 \\sim C62 \\sim C61: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C52: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C60, C59, C58, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C54, C55, C56, C57, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C46B(0.5) H46B(0.5) C47B(0.5) H47A(0.5) H47B(0.5) H47C(0.5)
 C46A(0.5) H46A(0.5) C47A(0.5) H47D(0.5) H47E(0.5) H47F(0.5) C48B(0.5)
 H48A(0.5) H48B(0.5) H48C(0.5) C48A(0.5) H48D(0.5) H48E(0.5) H48F(0.5) C60(0.5)
 H60(0.5) C59(0.5) H59(0.5) C58(0.5) H58(0.5) C63(0.5) H63(0.5) C62(0.5)
 H62(0.5) C61(0.5) H61(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5)
 H55(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C52(0.5) H52(0.5)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C33(H33), C11(H11), C46B(H46B), C8(H8), C46A(H46A)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C41(H41), C16(H16), C22(H22), C35(H35), C26(H26), C32(H32),
 C36(H36), C23(H23), C45(H45), C37(H37), C39(H39), C42(H42), C31(H31), C25(H25),
  C28(H28), C24(H24), C44(H44), C38(H38), C49(H49), C29(H29), C50(H50),
 C30(H30), C64(H64), C51(H51), C43(H43), C65(H65), C66(H66), C60(H60), C59(H59),
  C58(H58), C63(H63), C62(H62), C61(H61), C53(H53), C54(H54), C55(H55),
 C56(H56), C57(H57), C52(H52)
6.c Fitted hexagon refined as free rotating group:
 C60(C59,C58,C63,C62,C61)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C47B(H47A,H47B,
 H47C), C47A(H47D,H47E,H47F), C48B(H48A,H48B,H48C), C48A(H48D,H48E,H48F)
;
_shelx_res_checksum              61076
_olex2_submission_special_instructions 'No special instructions were received'