Isolation and reactivity of heteroleptic magnesium 1,3-benzazaphospholide complexes.
Pi, Chengfu; Zhou, Jie; Dalton transactions (Cambridge, England : 2003) 55 (2026) 2673–2680; doi:10.1039/d5dt03010b

data_7720051
_publ_section_title
;
 Isolation and reactivity of heteroleptic magnesium 1,3-benzazaphospholide
 complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2673
_journal_page_last               2680
_journal_paper_doi               10.1039/d5dt03010b
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C43 H52 Mg N3 P S2'
_chemical_formula_sum            'C43 H52 Mg N3 P S2'
_chemical_formula_weight         730.27
_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     dual
_audit_creation_date             2025-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-12-07 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.470(4)
_cell_length_b                   13.3630(15)
_cell_length_c                   15.7513(17)
_cell_measurement_reflns_used    6799
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.439
_cell_measurement_theta_min      2.504
_cell_volume                     8080.5(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20176
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.614
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7120
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0860
_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^)+(0.1305P)^2^+37.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5421
_reflns_number_total             7120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03010b2.cif
_cod_data_source_block           4a
_cod_original_cell_volume        8080.4(15)
_cod_database_code               7720051
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Restrained distances
 C7-N1 \\sim N1-C8
 with sigma of 0.02
2. Rigid bond restraints
 P1, C7
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 N1, C7
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
3. Uiso/Uaniso restraints and constraints
P1 \\sim N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within
3.8A with sigma of 0.005 and sigma for terminal atoms of 0.005 within 3.8A
4.a Ternary CH refined with riding coordinates:
 C16(H16), C24(H24), C35(H35), C42(H42)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C13(H13), C19(H19),
 C20(H20), C21(H21), C29(H29), C37(H37), C38(H38), C39(H39)
4.c Fitted hexagon refined as free rotating group:
 C6(C1,C2,C3,C4,C5)
4.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              37351
_shelx_hkl_checksum              51624
_olex2_submission_special_instructions 'No special instructions were received'