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_7720048
_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_absolute_configuration ad
_chemical_formula_moiety         'C47 H60 Mg N3 O P'
_chemical_formula_sum            'C47 H60 Mg N3 O P'
_chemical_formula_weight         738.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
_cell_angle_beta                 95.9250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8726(3)
_cell_length_b                   19.6268(4)
_cell_length_c                   18.8009(4)
_cell_measurement_reflns_used    7850
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.37
_cell_volume                     4357.60(17)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17742
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.013
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.9775
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.138
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2967 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7913
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0545P)^2^+0.2923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.853
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                7089
_reflns_number_total             7913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03010b2.cif
_cod_data_source_block           3a
_cod_database_code               7720048
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Others
 Sof(H30C)=Sof(H30D)=Sof(H33C)=Sof(H33D)=Sof(C42')=Sof(H42C)=Sof(H42D)=
 Sof(C46')=Sof(H46C)=Sof(H46D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H33A)=Sof(H33B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=FVAR(1)
2.a Riding coordinates:
 C15(H15), C17(H17), C19(H19), C21(H21), C41(H41A,H41B,H41C)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C30(H30C,H30D), C33(H33A,H33B), C33(H33C,H33D), C42(H42A,
 H42B), C42'(H42C,H42D), C46(H46A,H46B), C46'(H46C,H46D)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C13(H13), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
 C28(H28), C29(H29), C31(H31), C34(H34), C37(H37), C40(H40), C45(H45)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              40336
_shelx_hkl_checksum              12302
_olex2_submission_special_instructions 'No special instructions were received'