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_7720047
_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, 0.5(C7 H8)'
_chemical_formula_sum            'C46.5 H56 Mg N3 P'
_chemical_formula_weight         712.22
_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                78.932(2)
_cell_angle_beta                 73.301(2)
_cell_angle_gamma                73.616(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8701(15)
_cell_length_b                   12.3027(17)
_cell_length_c                   16.905(2)
_cell_measurement_reflns_used    7068
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.690
_cell_measurement_theta_min      2.271
_cell_volume                     2062.3(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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16358
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.281
_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_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7249
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0608P)^2^+1.0424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5609
_reflns_number_total             7249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03010b2.cif
_cod_data_source_block           2a
_cod_original_formula_sum        'C46.50 H56 Mg N3 P'
_cod_database_code               7720047
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Rigid bond restraints
 C44, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
2. Others
 Fixed Sof: C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C48(0.5) H48(0.5) C47(0.5)
 H47(0.5) C46(0.5) H46(0.5) C45(0.5) C50(0.5) H50(0.5) C49(0.5) H49(0.5)
3.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C33(H33), C36(H36)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C17(H17),
 C18(H18), C19(H19), C29(H29), C30(H30), C31(H31), C41(H41), C48(H48), C47(H47),
  C46(H46), C50(H50), C49(H49)
3.c Fitted hexagon refined as free rotating group:
 C48(C47,C46,C45,C50,C49)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C)
;
_shelx_res_checksum              93601
_shelx_hkl_checksum              55616
_olex2_submission_special_instructions 'No special instructions were received'