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_7713453
_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         '2(C21 H47 Cl Li Mg N3 O P2), C5 H12'
_chemical_formula_sum            'C47 H106 Cl2 Li2 Mg2 N6 O2 P4'
_chemical_formula_weight         1044.65
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-10
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-19 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                93.839(2)
_cell_angle_beta                 98.412(2)
_cell_angle_gamma                109.612(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7919(8)
_cell_length_b                   12.9748(9)
_cell_length_c                   22.3011(15)
_cell_measurement_reflns_used    4263
_cell_measurement_temperature    190.0
_cell_measurement_theta_max      26.774
_cell_measurement_theta_min      2.281
_cell_volume                     3154.7(4)
_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      190.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.997
_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  0.0898
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24096
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.928
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1421 before and 0.0832 after correction. The Ratio of minimum to maximum transmission is 0.7630. 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    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         11061
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0707P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6267
_reflns_number_total             11061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01657a2.cif
_cod_data_source_block           t-1_a
_cod_database_code               7713453
_shelxl_version_number           2013-2
_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
 C44-C45 = C47-C46 = C46-C43 = C45-C43
 1.55 with sigma of 0.01
 C45A-C44A \\sim C47-C46
 with sigma of 0.02
 C45A-C43A \\sim C46-C43
 with sigma of 0.02
 C46A-C43A \\sim C45-C43
 with sigma of 0.02
 C47A-C46A \\sim C45-C44
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C46A \\sim C47A \\sim C43A
\\sim C45A \\sim C44A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C45) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C43, C44, C45, C46, C47, C46A, C47A, C43A, C45A, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C44A)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=
 Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C9(H9), C12(H12), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B),
 C13(H13A,H13B), C23(H23A,H23B), C28(H28A,H28B), C29(H29A,H29B), C33(H33A,H33B),
  C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B),
 C46A(H46C,H46D), C43A(H43C,H43D), C45A(H45C,H45D)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C44(H44A,
 H44B,H44C), C47(H47A,H47B,H47C), C47A(H47D,H47E,H47F), C44A(H44D,H44E,H44F)
;
_shelx_res_checksum              34497
_olex2_submission_special_instructions 'No special instructions were received'