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_7713452
_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         'C34 H77 Au2 Cl2 Mg2 N6 P4'
_chemical_formula_sum            'C34 H77 Au2 Cl2 Mg2 N6 P4'
_chemical_formula_weight         1207.34
_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             2023-03-01
_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                78.19(5)
_cell_angle_beta                 87.56(4)
_cell_angle_gamma                65.18(7)
_cell_formula_units_Z            2
_cell_length_a                   12.441(18)
_cell_length_b                   13.95(3)
_cell_length_c                   16.13(3)
_cell_measurement_reflns_used    5906
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.826
_cell_measurement_theta_min      2.266
_cell_volume                     2484(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0720
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23756
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         1.862
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.193
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1386 before and 0.0678 after correction. The Ratio of minimum to maximum transmission is 0.7619. 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    1.615
_exptl_crystal_description       block
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         11309
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0365P)^2^+3.1117P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7163
_reflns_number_total             11309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01657a2.cif
_cod_data_source_block           t-2_a
_cod_original_cell_volume        2483(8)
_cod_database_code               7713452
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.371
_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
 C32-C34
 1.53 with sigma of 0.01
 N5-C33 \\sim N5-C33A
 with sigma of 0.02
 Cl1A-Mg2 \\sim Cl1-Mg2
 with sigma of 0.02
 Cl2-Mg2 \\sim Cl2A-Mg2
 with sigma of 0.02
 Cl1-Mg1 \\sim Cl1A-Mg1
 with sigma of 0.02
 Cl2-Mg1 \\sim Cl2A-Mg1
 with sigma of 0.02
3. Rigid bond restraints
 Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C12 \\sim N5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C33A \\sim C33: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Cl1 \\sim Cl2 \\sim Cl1A \\sim Cl2A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mg2, Mg1, Cl1, Cl2, Cl2A, Cl1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15), C19(H19)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C34(H34A,H34B), C32(H32A,H32B),
 C35(H35A,H35B), C28(H28A,H28B)
7.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), 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), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              2668
_olex2_submission_special_instructions 'No special instructions were received'