Magnesium Complexes Supported by Dianionic Double Layer Nitrogen-Phosphorus Ligand: Synthesis and Reactivity Study
Li, Yafei; Chen, Pengfei; Zhu, Qin; Zhu, Congqing; Dalton Transactions  (2023) –; doi:10.1039/D3DT01657A

data_7713451
_publ_section_title
;
 Magnesium Complexes Supported by Dianionic Double Layer
 Nitrogen-Phosphorus Ligand: Synthesis and Reactivity Study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01657A
_journal_year                    2023
_chemical_formula_moiety         'C17 H39 Ag I Mg N3 P2'
_chemical_formula_sum            'C17 H39 Ag I Mg N3 P2'
_chemical_formula_weight         606.53
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-03-19 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.704(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.870(3)
_cell_length_b                   14.5992(17)
_cell_length_c                   14.7309(16)
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.156
_cell_measurement_theta_min      2.923
_cell_volume                     5116.2(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      190.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24208
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.790
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1512 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.8515. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5869
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0295P)^2^+6.8050P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3917
_reflns_number_total             5869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01657a2.cif
_cod_data_source_block           t_a_CCDC2
_cod_database_code               7713451
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.649
_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
 C6-C16
 1.55 with sigma of 0.01
 C9A-C14A = C9-C14 = C9-C17 = C9A-C17A
 1.54 with sigma of 0.01
 P2-C8A \\sim P2-C8
 with sigma of 0.02
 C8A-C15A \\sim C8-C15
 with sigma of 0.02
 C8A-C12A \\sim C8-C12
 with sigma of 0.02
 C9A-C14A \\sim C9-C14
 with sigma of 0.02
 P2-C9 \\sim P2-C9A
 with sigma of 0.02
 C9-C17 \\sim C9A-C17A
 with sigma of 0.02
 C6-C13A \\sim C6-C13
 with sigma of 0.02
 C6-C16 \\sim C6-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim C8 \\sim C9 \\sim C12 \\sim C14 \\sim C15 \\sim C17 \\sim C8A \\sim
C12A \\sim C15A \\sim C9A \\sim C17A \\sim C14A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C9) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 P2, C8, C12, C15, C8A, C12A, C15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P2, C9, C14, C17, C9A, C17A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C6, C13, C16, C13A, C16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C8A)=Sof(H8A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C9A)=Sof(H9A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C9)=Sof(H9)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(H6B)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=1-FVAR(3)
 Sof(H6A)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C6(H6A), C6(H6B), C8(H8), C9(H9), C8A(H8A), C9A(H9A)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C12A(H12D,H12E,H12F), C15A(H15D,H15E,H15F),
 C17A(H17D,H17E,H17F), C14A(H14D,H14E,H14F), C13A(H13D,H13E,H13F), C16A(H16D,
 H16E,H16F)
;
_shelx_res_checksum              97718
_olex2_submission_special_instructions 'No special instructions were received'