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_7720671
_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 Co N3 O3 P3, 2(C24 H20 B), C4 H10 O'
_chemical_formula_sum            'C97 H98 B2 Co N3 O4 P3'
_chemical_formula_weight         1543.24
_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     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                117.7140(10)
_cell_angle_beta                 106.0810(10)
_cell_angle_gamma                97.3950(10)
_cell_formula_units_Z            2
_cell_length_a                   16.13080(10)
_cell_length_b                   18.2809(2)
_cell_length_c                   18.4056(2)
_cell_measurement_reflns_used    66882
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.9100
_cell_measurement_theta_min      2.2710
_cell_volume                     4400.22(10)
_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      100.00(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 0.880
_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     -6.00  20.00   0.50    1.54    --   13.07  75.00-137.25   52
  2  \w     -5.00  22.00   0.50    1.54    --   13.07  74.00 -73.97   54
  3  \w      2.00  56.00   0.50    1.54    --   13.07  57.00   0.00  108
  4  \w     -5.00  25.00   0.50    1.54    --   13.07  73.00  75.20   60
  5  \w      2.00  56.00   0.50    1.54    --   13.07  57.00 150.00  108
  6  \w     16.00  91.00   0.50    1.54    --   13.07  19.00  90.00  150
  7  \w      7.00  88.00   0.50    1.54    --   13.07  38.00   0.00  162
  8  \w      7.00  88.00   0.50    1.54    --   13.07  38.00   0.00  162
  9  \w      7.00  88.00   0.50    1.54    --   13.07  38.00 -90.00  162
 10  \w    -67.00 -25.00   0.50    1.54    --  -14.48 138.00 -34.60   84
 11  \w     16.00  64.00   0.50    1.54    --  -14.48  19.00-120.00   96
 12  \w     16.00  64.00   0.50    1.54    --  -14.48  19.00 120.00   96
 13  \w    -65.00 -22.00   0.50    1.54    --   13.07 -19.00 120.00   86
 14  \w    -65.00 -22.00   0.50    1.54    --   13.07 -19.00 150.00   86
 15  \w    -60.00  25.00   0.50    1.54    --   13.07 -57.00 -30.00  170
 16  \w    -24.00  33.00   0.50    1.54    --   13.07 -77.00-120.00  114
 17  \w    -24.00  33.00   0.50    1.54    --   13.07 -77.00-180.00  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      -0.0013099000
_diffrn_orient_matrix_UB_12      0.0020072000
_diffrn_orient_matrix_UB_13      -0.0378564000
_diffrn_orient_matrix_UB_21      0.0214982000
_diffrn_orient_matrix_UB_22      0.0453906000
_diffrn_orient_matrix_UB_23      0.0275924000
_diffrn_orient_matrix_UB_31      0.0429142000
_diffrn_orient_matrix_UB_32      -0.0071000000
_diffrn_orient_matrix_UB_33      0.0052597000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            132450
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.934
_diffrn_reflns_theta_min         2.273
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60669
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1044
_refine_ls_number_reflns         29045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0866P)^2^+2.0727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22502
_reflns_number_total             29045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2024rk_ksexp1pink_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_original_cell_volume        4400.22(8)
_cod_database_code               7720671
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co N P O H C B'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.905
_diffrn_oxdiff_ac3_digest_hkl    0165a5534b1fc54c66bde2b9adfd8f2e559d9b
_diffrn_oxdiff_digest_hkl
;
43d28a18433246cdf02cd5b83b074447e1f416
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: O4(0.5) O5(0.5) C100(0.5) H10A(0.5) H10B(0.5) C99(0.5) H99A(0.5)
 H99B(0.5) C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5) C101(0.5) H10C(0.5) H10D(0.5)
 H10E(0.5) C95(0.5) H95A(0.5) H95B(0.5) C96(0.5) H96A(0.5) H96B(0.5) C98(0.5)
 H98A(0.5) H98B(0.5) H98C(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C28(H28A,H28B), C29(H29A,H29B), C42(H42A,H42B), C43(H43A,
 H43B), C31(H31A,H31B), C13(H13A,H13B), C15(H15A,H15B), C30(H30A,H30B),
 C100(H10A,H10B), C99(H99A,H99B), C95(H95A,H95B), C96(H96A,H96B)
2.b Aromatic/amide H refined with riding coordinates:
 C72(H72), C71(H71), C83(H83), C81(H81), C73(H73), C75(H75), C79(H79),
 C87(H87), C78(H78), C74(H74), C80(H80), C21(H21), C6(H6), C65(H65), C27(H27),
 C86(H86), C84(H84), C66(H66), C7(H7), C26(H26), C93(H93), C8(H8), C51(H51),
 C11(H11), C85(H85), C45(H45), C89(H89), C63(H63), C59(H59), C92(H92), C2(H2),
 C20(H20), C62(H62), C9(H9), C23(H23), C25(H25), C17(H17), C4(H4), C10(H10),
 C50(H50), C60(H60), C5(H5), C3(H3), C41(H41), C49(H49), C35(H35), C61(H61),
 C67(H67), C24(H24), C53(H53), C32(H32), C90(H90), C91(H91), C19(H19), C69(H69),
  C37(H37), C47(H47), C57(H57), C18(H18), C68(H68), C54(H54), C33(H33),
 C56(H56), C55(H55), C48(H48), C34(H34), C40(H40), C39(H39), C38(H38)
2.c Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C101(H10C,H10D,H10E), C98(H98A,H98B,H98C), C97(H97A,H97B,
 H97C)
;
_shelx_res_checksum              38160
_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 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.541