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_7720050
_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         'C42 H50 Mg N3 P, 0.5(C7 H8)'
_chemical_formula_sum            'C45.5 H54 Mg N3 P'
_chemical_formula_weight         698.19
_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             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                91.558(2)
_cell_angle_beta                 96.792(2)
_cell_angle_gamma                105.766(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0667(15)
_cell_length_b                   11.3787(17)
_cell_length_c                   18.648(3)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.419
_cell_measurement_theta_min      2.223
_cell_volume                     2037.3(5)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16231
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         1.102
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0690P)^2^+0.3236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6749
_reflns_number_total             8630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03010b2.cif
_cod_data_source_block           2b
_cod_original_formula_sum        'C45.50 H54 Mg N3 P'
_cod_database_code               7720050
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C44 \\sim C43 \\sim C48 \\sim C45 \\sim C49 \\sim C47 \\sim C46: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C47) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C46) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23A)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=FVAR(1)
 Fixed Sof: C47(0.5) H47(0.5) C48(0.5) H48(0.5) C43(0.5) H43(0.5) C44(0.5)
 C45(0.5) H45(0.5) C46(0.5) H46(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C23(H23), C26(H26), C23A(H23A)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C15(H15), C19(H19), C20(H20), C21(H21), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C47(H47), C48(H48), C43(H43), C45(H45), C46(H46)
3.c Fitted hexagon refined as free rotating group:
 C47(C48,C43,C44,C45,C46)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C49(H49A,H49B,H49C),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              15460
_shelx_hkl_checksum              77692
_olex2_submission_special_instructions 'No special instructions were received'