Unsymmetrical bis(anilido)xanthene ligands: development and use in the preparation of magnesium diamide complexes.
Evans, Matthew J.; Jones, Cameron; Chemical communications (Cambridge, England) 61 (2025) 11814–11817; doi:10.1039/d5cc03202d

data_7134775
_publ_section_title
;
 Unsymmetrical bis(anilido)xanthene ligands: development and use in the
 preparation of magnesium diamide complexes.
;
_journal_issue                   63
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11814
_journal_page_last               11817
_journal_paper_doi               10.1039/d5cc03202d
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C43 H58 N2 O'
_chemical_formula_sum            'C43 H58 N2 O'
_chemical_formula_weight         618.91
_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     fmap
_audit_creation_date             2025-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-06-05 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                103.3550(10)
_cell_angle_beta                 102.2380(10)
_cell_angle_gamma                103.6610(10)
_cell_formula_units_Z            4
_cell_length_a                   9.99070(10)
_cell_length_b                   17.0201(2)
_cell_length_c                   23.3184(2)
_cell_measurement_reflns_used    50957
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.7400
_cell_measurement_theta_min      3.8950
_cell_volume                     3596.71(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'w\ scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.360
_diffrn_reflns_theta_min         3.914
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         15546
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0693P)^2^+2.3590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13710
_reflns_number_total             15546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03202d2.cif
_cod_data_source_block           cj1743
_cod_depositor_comments
'Adding full bibliography for 7134774--7134781.cif.'
_cod_database_code               7134775
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Restrained distances
 C28-C90
 1.52 with sigma of 0.01
 C90-C89
 1.54 with sigma of 0.01
 C39-C38
 1.54 with sigma of 0.01
 C28-C39
 1.52 with sigma of 0.01
 C87-C88
 1.54 with sigma of 0.01
 C88-C77
 1.52 with sigma of 0.01
 C85-C86
 1.54 with sigma of 0.01
 C86-C77
 1.52 with sigma of 0.01
 C90-C29 = C90-C27
 2.52 with sigma of 0.005
 C39-C29 = C39-C27
 2.52 with sigma of 0.005
 C28-C26
 2.42 with sigma of 0.01
 C28-C30
 2.41 with sigma of 0.01
 C86-C78
 2.52 with sigma of 0.04
 C88-C76
 2.52 with sigma of 0.04
 C88-C78
 2.52 with sigma of 0.04
 C86-C76
 2.52 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C28 \\sim C90 \\sim C89: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C28 \\sim C39 \\sim C38: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C77 \\sim C86 \\sim C85 \\sim C87 \\sim C88: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C85) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C28, C90, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C77, C86, C85, C87, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C89)=Sof(H33)=Sof(H34)=Sof(H35)=Sof(C90)=Sof(H31)=Sof(H32)=1-FVAR(1)
 Sof(C38)=Sof(H28)=Sof(H29)=Sof(H30)=Sof(C39)=Sof(H26)=Sof(H27)=FVAR(1)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=Sof(H88B)=1-FVAR(2)
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C86)=Sof(H86A)=Sof(H86B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C7(HC), C13(HF), C19(HB), C50(H50), C56(H56), C62(H62)
5.b Secondary CH2 refined with riding coordinates:
 C8(HN,HO), C9(H9,H10), C10(H13,H14), C11(H5,H6), C12(HJ,HK), C14(H15,H16),
 C15(H20,H21), C16(H24,H25), C17(H22,H23), C18(H11,H12), C20(HH,HI), C21(H2,H4),
  C22(HY,HZ), C23(HW,HX), C24(HL,HM), C39(H26,H27), C43(H7,H8), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,
 H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
 C82(H82A,H82B), C86(H86A,H86B), C88(H88A,H88B), C90(H31,H32)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H), N3(H3), C3(HE), C5(HA), C27(HV), C29(H1), C33(HG), C35(HD), C46(H46),
 C48(H48), C70(H70), C72(H72), C76(H76), C78(H78)
5.d Idealised Me refined as rotating group:
 C38(H28,H29,H30), C40(HS,HT,HU), C41(HP,HQ,HR), C42(H17,H18,H19), C81(H81A,
 H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C),
 C87(H87A,H87B,H87C), C89(H33,H34,H35)
;
_shelx_res_checksum              31010
_shelx_hkl_checksum              15712
_olex2_submission_special_instructions 'No special instructions were received'