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_7713449
_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 H82 Mg2 N8 Na2 P4'
_chemical_formula_sum            'C34 H82 Mg2 N8 Na2 P4'
_chemical_formula_weight         821.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 114.657(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9772(6)
_cell_length_b                   15.3074(7)
_cell_length_c                   13.8680(6)
_cell_measurement_reflns_used    4071
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      45.569
_cell_measurement_theta_min      3.412
_cell_volume                     2503.7(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      193.00
_diffrn_measured_fraction_theta_full 0.998
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.961
_diffrn_reflns_theta_min         3.411
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1357 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.8959. 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    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0671P)^2^+0.4758P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2561
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01657a2.cif
_cod_data_source_block           t_a
_cod_database_code               7713449
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.778
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C16(H16), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C8(H8A,H8B), C7(H7A,H7B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C4(H4C,H4D,H4E), C14(H14A,H14B,H14C),
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              31621
_olex2_submission_special_instructions 'No special instructions were received'