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_7720049
_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         'C46 H58 Mg N3 O P, 0.5(C4 H8 O)'
_chemical_formula_sum            'C48 H62 Mg N3 O1.5 P'
_chemical_formula_weight         760.28
_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             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                82.510(2)
_cell_angle_beta                 81.711(2)
_cell_angle_gamma                69.129(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1505(5)
_cell_length_b                   12.2547(5)
_cell_length_c                   17.4420(7)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.22
_cell_volume                     2195.67(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31142
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.785
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.8932
_exptl_absorpt_correction_T_min  0.8640
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.9773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6531
_reflns_number_total             7717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03010b2.cif
_cod_data_source_block           3b
_cod_original_formula_sum        'C48 H62 Mg N3 O1.50 P'
_cod_database_code               7720049
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Restrained distances
 C50-O2 = O2-C49
 1.4 with sigma of 0.02
 C48-C47
 1.5 with sigma of 0.02
 C50-C48 = C47-C49
 1.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C47 \\sim O2 \\sim C49 \\sim C50 \\sim C48: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: O2(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C42(H42A,H42B), C43(H43A,H43B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C18(H18), C19(H19), C21(H21), C23(H23),
 C25(H25), C27(H27), C28(H28), C30(H30), C32(H32), C33(H33), C35(H35), C40(H40)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              42631
_shelx_hkl_checksum              49869
_olex2_submission_special_instructions 'No special instructions were received'