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_7720667
_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         'C54 H59 N4 O3 P3, C2 H3 N'
_chemical_formula_sum            'C56 H62 N5 O3 P3'
_chemical_formula_weight         946.01
_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
_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                76.1760(10)
_cell_angle_beta                 79.8520(10)
_cell_angle_gamma                62.7780(10)
_cell_formula_units_Z            2
_cell_length_a                   12.82860(10)
_cell_length_b                   12.83880(10)
_cell_length_c                   17.7410(2)
_cell_measurement_reflns_used    92989
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.5510
_cell_measurement_theta_min      1.9540
_cell_volume                     2515.53(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9196
_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    -57.00  -5.00   0.50    5.00    --  -16.31 116.00 134.00  104
  2  \w     11.00  60.00   0.50    5.00    --   19.28-116.00  46.00   98
  3  \w    -56.00  -2.00   0.50    5.00    --  -16.31 -57.00 -90.00  108
  4  \w    -56.00  -2.00   0.50    5.00    --  -16.31 -57.00-180.00  108
  5  \w     21.00  63.00   0.50    5.00    --  -16.31  19.00  90.00   84
  6  \w     21.00  63.00   0.50    5.00    --  -16.31  19.00-150.00   84
  7  \w      5.00  62.00   0.50    5.00    --   19.28  57.00 -90.00  114
  8  \w     -4.00  23.00   0.50    5.00    --   19.28  78.00  48.10   54
  9  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00 -30.00   86
 10  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00 -60.00   86
 11  \w     -4.00  23.00   0.50    5.00    --   19.28  78.00-132.09   54
 12  \w      5.00  62.00   0.50    5.00    --   19.28  57.00   0.00  114
 13  \w     -4.00  24.00   0.50    5.00    --   19.28  77.00-158.00   56
 14  \w      5.00  62.00   0.50    5.00    --   19.28  57.00 120.00  114
 15  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00 -90.00   86
 16  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00   0.00   86
 17  \w      0.00  52.00   0.50    5.00    --   19.28 -99.00   0.00  104
 18  \w     -5.00  21.00   0.50    5.00    --   19.28  80.00-173.54   52
 19  \w      0.00  52.00   0.50    5.00    --   19.28 -99.00  30.00  104
 20  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00  90.00   86
 21  \w    -53.00   2.00   0.50    5.00    --  -16.31 105.00   1.58  110
 22  \w    -72.00 -20.00   0.50    5.00    --  -16.31 139.00  67.28  104
 23  \w     21.00  63.00   0.50    5.00    --  -16.31  19.00-120.00   84
 24  \w    -71.00 -18.00   0.50    5.00    --  -16.31 136.00 -70.83  106
 25  \w    -46.00  12.00   0.50    5.00    --  -16.31  91.00-150.35  116
 26  \w    -45.00  13.00   0.50    5.00    --  -16.31  90.00-121.75  116
 27  \w    -71.00 -18.00   0.50    5.00    --  -16.31 136.00 147.56  106
 28  \w      0.00  52.00   0.50    5.00    --   19.28 -99.00 -30.00  104
 29  \w     -5.00  22.00   0.50    5.00    --   19.28  79.00 126.48   54
 30  \w    -18.00  42.00   0.50    5.00    --   19.28 -77.00 -90.00  120
 31  \w      5.00  97.00   0.50    5.00    --   19.28  38.00-150.00  184
 32  \w     -4.00  24.00   0.50    5.00    --   19.28  77.00 -82.19   56
 33  \w     -3.00  24.00   0.50    5.00    --   19.28  76.00  90.28   54
 34  \w    -18.00  42.00   0.50    5.00    --   19.28 -77.00  60.00  120
 35  \w     -5.00  50.00   0.50    5.00    --   19.28 -92.00 116.49  110
 36  \w      5.00  97.00   0.50    5.00    --   19.28  38.00  30.00  184
 37  \w    -53.00   2.00   0.50    5.00    --  -16.31 105.00  98.31  110
 38  \w    -71.00 -20.00   0.50    5.00    --  -16.31 136.00  15.11  102
 39  \w    -49.00   7.00   0.50    5.00    --  -16.31  98.00 -90.99  112
 40  \w     21.00  99.00   0.50    5.00    --   19.28  19.00 -60.00  156
 41  \w    -60.00 -17.00   0.50    5.00    --   19.28 -19.00 150.00   86
;
_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      -0.0262915000
_diffrn_orient_matrix_UB_12      0.0621258000
_diffrn_orient_matrix_UB_13      -0.0001589000
_diffrn_orient_matrix_UB_21      0.0038246000
_diffrn_orient_matrix_UB_22      -0.0114201000
_diffrn_orient_matrix_UB_23      0.0408022000
_diffrn_orient_matrix_UB_31      0.0564218000
_diffrn_orient_matrix_UB_32      -0.0006160000
_diffrn_orient_matrix_UB_33      -0.0063762000
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            162859
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.604
_diffrn_reflns_theta_min         1.791
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
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    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         18282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0401P)^2^+2.0366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15989
_reflns_number_total             18282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025_nks_9740_03mecn_auto_1
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P '
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.979
_diffrn_oxdiff_ac3_digest_hkl    019823867a0f18dd29176002fedef28bce97d4
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C31(H31A,H31B), C13(H13A,H13B), C30(H30A,H30B), C16(H16A,
 H16B), C44(H44A,H44B), C15(H15A,H15B), C54(H54A,H54B), C45(H45A,H45B),
 C29(H29A,H29B), C46(H46A,H46B), C53(H53A,H53B)
1.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C12(H12), C39(H39), C48(H48), C22(H22), C6(H6), C37(H37), C42(H42),
 C8(H8), C33(H33), C2(H2), C18(H18), C11(H11), C52(H52), C40(H40), C3(H3),
 C28(H28), C34(H34), C49(H49), C10(H10), C41(H41), C24(H24), C21(H21), C36(H36),
  C9(H9), C4(H4), C20(H20), C5(H5), C35(H35), C51(H51), C19(H19), C50(H50),
 C25(H25), C27(H27), C26(H26)
1.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C)
;
_shelx_res_checksum              20188
_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 2.739
_oxdiff_exptl_absorpt_empirical_full_min 0.605