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_7713448
_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         'C19 H45 I Mg N3 P2, I'
_chemical_formula_sum            'C19 H45 I2 Mg N3 P2'
_chemical_formula_weight         655.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 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                 110.85(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.868(3)
_cell_length_b                   15.384(5)
_cell_length_c                   14.660(9)
_cell_measurement_reflns_used    1783
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.65
_cell_volume                     2923(2)
_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      296.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11066
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.990
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5599
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0825 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.7509.
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    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0177P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2120
_reflns_number_total             4085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01657a2.cif
_cod_data_source_block           t-3_a
_cod_database_code               7713448
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.04(4)
 -0.04(4)
2. 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
3. Restrained distances
 C6A-C5A = C6-C5 = C6-C4 = C6A-C4A = C2-C1 = C2A-C1A = C3A-C2A = C3-C2
 1.54 with sigma of 0.001
 C19-C17 = C18-C17 = C15-C14 = C14-C13
 1.54 with sigma of 0.001
 C9-C8
 1.54 with sigma of 0.001
 P1A-N1 \\sim P1-N1
 with sigma of 0.02
 C6A-C5A \\sim C6-C5
 with sigma of 0.02
 P1A-C2A \\sim P1-C2
 with sigma of 0.02
 P1A-C6A \\sim P1-C6
 with sigma of 0.02
 C3A-C2A \\sim C3-C2
 with sigma of 0.02
 C6A-C4A \\sim C6-C4
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 P1A-C7A \\sim P1-C7
 with sigma of 0.02
 C3A-C1A \\sim C3-C1
 with sigma of 0.02
 P1A-C1 \\sim P1A-C1A
 with sigma of 0.02
 P2-C14A \\sim P2-C14
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 C14A-C13A \\sim C14-C13
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
P1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim P1A
\\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P2 \\sim C13 \\sim C14 \\sim C15 \\sim C14A \\sim C13A \\sim C15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 P1, C1, C2, C3, C4, C5, C6, C7, P1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P2, C13, C14, C15, C14A, C13A, C15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(P1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=
 Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=1-FVAR(1)
 Sof(P1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(C14A)=Sof(H14A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C15A)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(2)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C2(H2), C6(H6), C2A(H2A), C6A(H6A), C14A(H14A)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B)
7.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C1A(H1AA,H1AB,H1AC),
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C7A(H7AA,H7AB,
 H7AC), C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              7628
_olex2_submission_special_instructions 'No special instructions were received'