Transition metal complexes with phosphine oxide appended aza-macrocycles - effects of ring size and denticity.
Herniman, Julie M.; P Keeling, George; King, Rhys P.; Light, Mark E.; Kandathil Sintho, Navya; Snowsill, Kate; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5266–5275; doi:10.1039/d6dt00255b

data_7720674
_publ_section_title
;
 Transition metal complexes with phosphine oxide appended aza-macrocycles
 - effects of ring size and denticity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5266
_journal_page_last               5275
_journal_paper_doi               10.1039/d6dt00255b
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C45 H48 N3 Ni O3 P3, 2(C24 H20 B), C4 H10 O'
_chemical_formula_sum            'C97 H98 B2 N3 Ni O4 P3'
_chemical_formula_weight         1543.02
_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     dual
_audit_creation_date             2025-08-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-12-15 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                117.583(2)
_cell_angle_beta                 97.1660(10)
_cell_angle_gamma                105.699(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0832(3)
_cell_length_b                   18.3082(3)
_cell_length_c                   18.3795(3)
_cell_measurement_reflns_used    52751
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.4240
_cell_measurement_theta_min      2.1990
_cell_volume                     4415.17(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     12.00  58.00   0.50   21.77    --   13.07-127.00-142.00   92
  2  \w      2.00  56.00   0.50   21.77    --   13.07  57.00-180.00  108
  3  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00 120.00   86
  4  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00  60.00   86
  5  \w     -3.00  30.00   0.50   21.77    --   13.07  70.00 125.60   66
  6  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00-180.00   86
  7  \w     -6.00  20.00   0.50   21.77    --   13.07  75.00-105.55   52
  8  \w     -5.00  22.00   0.50   21.77    --   13.07  74.00 143.62   54
  9  \w      2.00  56.00   0.50   21.77    --   13.07  57.00   0.00  108
 10  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00 -90.00   86
 11  \w     -6.00  20.00   0.50   21.77    --   13.07  75.00 -67.33   52
 12  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00 -30.00   86
 13  \w      2.00  56.00   0.50   21.77    --   13.07  57.00  90.00  108
 14  \w     -6.00  43.00   0.50   21.77    --   13.07 -99.00 -90.00   98
 15  \w    -65.00 -22.00   0.50   21.77    --   13.07 -19.00   0.00   86
 16  \w    -34.00  18.00   0.50   21.77    --  -14.48  77.00   0.00  104
 17  \w    -34.00  18.00   0.50   21.77    --  -14.48  77.00-120.00  104
 18  \w     16.00  64.00   0.50   21.77    --  -14.48  19.00 120.00   96
 19  \w    -34.00  18.00   0.50   21.77    --  -14.48  77.00  30.00  104
 20  \w    -62.00  -3.00   0.50   21.77    --  -14.48 -57.00   0.00  118
 21  \w    -24.00  33.00   0.50   21.77    --   13.07 -77.00 150.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138990000
_diffrn_orient_matrix_UB_12      0.0324514000
_diffrn_orient_matrix_UB_13      -0.0114612000
_diffrn_orient_matrix_UB_21      -0.0154514000
_diffrn_orient_matrix_UB_22      -0.0340203000
_diffrn_orient_matrix_UB_23      -0.0439878000
_diffrn_orient_matrix_UB_31      -0.0431722000
_diffrn_orient_matrix_UB_32      0.0030992000
_diffrn_orient_matrix_UB_33      -0.0027567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            132615
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.867
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.141a (Rigaku Oxford Diffraction, 2024)
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    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.961
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         29193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1053P)^2^+3.9658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22144
_reflns_number_total             29193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2024rk_ksexp2_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_original_cell_volume        4415.16(16)
_cod_database_code               7720674
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni B C P O N C H'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.953
_diffrn_oxdiff_ac3_digest_hkl    017193f375d58a428667334de7e5644de1785e
_diffrn_oxdiff_digest_hkl
;
437b37f70691b505ac435da90b9b2040399e87
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: O5(0.5) C98(0.5) H98A(0.5) H98B(0.5) H98C(0.5) C99(0.5) H99A(0.5)
 H99B(0.5) C100(0.5) H10A(0.5) H10B(0.5) C101(0.5) H10C(0.5) H10D(0.5)
 H10E(0.5) O4(0.5) C94(0.5) H94A(0.5) H94B(0.5) C96(0.5) H96A(0.5) H96B(0.5)
 C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C45(H45A,H45B), C16(H16A,H16B), C13(H13A,H13B), C44(H44A,
 H44B), C30(H30A,H30B), C14(H14A,H14B), C29(H29A,H29B), C15(H15A,H15B),
 C99(H99A,H99B), C100(H10A,H10B), C94(H94A,H94B), C96(H96A,H96B)
2.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C57(H57), C65(H65), C68(H68), C69(H69), C50(H50), C59(H59),
 C63(H63), C49(H49), C47(H47), C53(H53), C8(H8), C89(H89), C36(H36), C42(H42),
 C48(H48), C67(H67), C66(H66), C90(H90), C6(H6), C40(H40), C54(H54), C9(H9),
 C56(H56), C38(H38), C83(H83), C55(H55), C2(H2), C39(H39), C84(H84), C41(H41),
 C60(H60), C12(H12), C62(H62), C24(H24), C32(H32), C35(H35), C33(H33), C34(H34),
  C18(H18), C91(H91), C10(H10), C61(H61), C3(H3), C71(H71), C25(H25), C81(H81),
 C5(H5), C75(H75), C77(H77), C22(H22), C11(H11), C28(H28), C26(H26), C92(H92),
 C72(H72), C93(H93), C4(H4), C80(H80), C74(H74), C79(H79), C85(H85), C27(H27),
 C87(H87), C73(H73), C78(H78), C21(H21), C86(H86), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C), C101(H10C,H10D,H10E), C95(H95A,H95B,H95C), C97(H97A,H97B,
 H97C)
;
_shelx_res_checksum              33501
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.077
_oxdiff_exptl_absorpt_empirical_full_min 0.469