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_1573702
_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 H112 Mg2 N4 Ni O2 P2'
_chemical_formula_sum            'C96 H113 Mg2 N4 Ni O2 P2'
_chemical_formula_weight         1524.17
_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
_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                110.227(3)
_cell_angle_beta                 101.922(4)
_cell_angle_gamma                108.780(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0759(14)
_cell_length_b                   18.5965(17)
_cell_length_c                   20.2198(16)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      56.87
_cell_measurement_theta_min      2.44
_cell_volume                     4702.6(8)
_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      120.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108633
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.312
_diffrn_reflns_theta_min         2.884
_diffrn_source_current           3.57
_diffrn_source_power             0.2494002
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1526 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.8252.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         19250
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0884P)^2^+1.3832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13971
_reflns_number_total             19250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03495c2.cif
_cod_data_source_block           ga220920b_0m_a
_cod_depositor_comments
'Adding full bibliography for 1573698--1573702.cif.'
_cod_original_cell_volume        4702.6(7)
_cod_database_code               1573702
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C2-H2A
 1 with sigma of 0.02
 Mg1-H2A
 2.53 with sigma of 0.04
2.a Ternary CH refined with riding coordinates:
 C71(H71), C25(H25), C38(H38), C68(H68), C84(H84), C59(H59), C10(H10),
 C22(H22), C56(H56), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C20(H20), C66(H66), C83(H83), C18(H18), C77(H77), C46(H46),
 C90(H90), C73(H73), C31(H31), C82(H82), C81(H81), C96(H96), C79(H79), C40(H40),
  C47(H47), C80(H80), C76(H76), C92(H92), C41(H41), C75(H75), C86(H86),
 C27(H27), C30(H30), C94(H94), C44(H44), C50(H50), C33(H33), C48(H48), C74(H74),
  C37(H37), C29(H29), C89(H89), C95(H95), C93(H93), C49(H49), C88(H88),
 C42(H42), C28(H28), C87(H87), C36(H36), C35(H35), C43(H43), C34(H34)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C60(H60A,H60B,
 H60C), C24(H24A,H24B,H24C), C7(H7A,H7B,H7C), C69(H69A,H69B,H69C), C57(H57A,
 H57B,H57C), C11(H11A,H11B,H11C), C61(H61A,H61B,H61C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15119
_shelx_fab_checksum              1686
_olex2_submission_special_instructions 'No special instructions were received'