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_7720668
_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
'2(C41 H46 Co N4 O2 P2), 4(C24 H20 B), 2(C H1.5 N0.5)'
_chemical_formula_sum            'C180 H175 B4 Co2 N9 O4 P4'
_chemical_formula_weight         2813.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 105.9370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4741(2)
_cell_length_b                   35.5051(4)
_cell_length_c                   16.4405(2)
_cell_measurement_reflns_used    103728
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.0590
_cell_measurement_theta_min      1.8390
_cell_volume                     7562.82(17)
_computing_cell_refinement       'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_computing_data_collection       'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_computing_data_reduction        'CrysAlisPro 1.171.44.96a (Rigaku OD, 2025)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.933
_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      9.00  61.06   0.38   15.00    --   17.09-122.00  89.00  137
  2  \w    -63.00 -15.88   0.38   15.00    --  -18.50 122.00 171.00  124
  3  \w    -62.00 -22.86   0.38   15.00    --   17.09 -19.00  90.00  103
  4  \w    -62.00 -22.86   0.38   15.00    --   17.09 -19.00   0.00  103
  5  \w     -3.00  28.92   0.38   15.00    --   17.09  71.00-103.19   84
  6  \w      3.00  55.06   0.38   15.00    --   17.09  57.00-180.00  137
  7  \w     -3.00  28.92   0.38   15.00    --   17.09  70.00 -84.23   84
  8  \w     -4.00  21.08   0.38   15.00    --   17.09  74.00 104.67   66
  9  \w     16.00  61.22   0.38   15.00    --  -18.50  19.00-120.00  119
 10  \w    -73.00 -24.74   0.38   15.00    --  -18.50 136.00  65.06  127
 11  \w     16.00  61.22   0.38   15.00    --  -18.50  19.00-150.00  119
 12  \w     16.00  61.22   0.38   15.00    --  -18.50  19.00 120.00  119
 13  \w      3.00  55.06   0.38   15.00    --   17.09  57.00 120.00  137
 14  \w    -62.00 -22.86   0.38   15.00    --   17.09 -19.00 -30.00  103
 15  \w      3.00  55.06   0.38   15.00    --   17.09  57.00  30.00  137
 16  \w     -4.00  21.08   0.38   15.00    --   17.09  74.00 132.82   66
 17  \w      3.00  55.06   0.38   15.00    --   17.09  57.00 -60.00  137
 18  \w     16.00  61.22   0.38   15.00    --  -18.50  19.00 150.00  119
 19  \w    -48.00   6.34   0.38   15.00    --  -18.50  90.00 -84.10  143
 20  \w    -41.00  17.14   0.38   15.00    --  -18.50  77.00-150.00  153
 21  \w    -45.00  10.10   0.38   15.00    --  -18.50  84.00  54.22  145
 22  \w     16.00  61.22   0.38   15.00    --  -18.50  19.00 -60.00  119
 23  \w    -98.00 -22.00   0.38   15.00    --  -18.50 -19.00 120.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0299338000
_diffrn_orient_matrix_UB_12      0.0129093000
_diffrn_orient_matrix_UB_13      0.0162365000
_diffrn_orient_matrix_UB_21      -0.0196508000
_diffrn_orient_matrix_UB_22      -0.0150861000
_diffrn_orient_matrix_UB_23      0.0192391000
_diffrn_orient_matrix_UB_31      0.0414266000
_diffrn_orient_matrix_UB_32      0.0021808000
_diffrn_orient_matrix_UB_33      0.0371277000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            247513
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.393
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.96a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         27432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0596P)^2^+8.4295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23130
_reflns_number_total             27432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_cobnnodpph_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720668
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co N H P O B C'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.969
_diffrn_oxdiff_ac3_digest_hkl    017a7b0272d72cbab613a256dafc7902e65200
_diffrn_oxdiff_digest_hkl
;
43590c1b858c98602174d1688598bc45fd5757
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Others
 Fixed Sof: C89(0.5) H89C(0.25) H89B(0.25) H89A(0.25) H89F(0.25) H89E(0.25)
 H89D(0.25) C90(0.25) N6(0.25) C91(0.25) N5(0.25) C22A(0.5) C23(0.5) H23(0.5)
 C27A(0.5) H27A(0.5) C26A(0.5) H26A(0.5) C24(0.5) H24(0.5) C25A(0.5) H25A(0.5)
 C25(0.5) H25(0.5) C24A(0.5) H24A(0.5) C27(0.5) H27(0.5) C26(0.5) H26(0.5)
 C23A(0.5) H23A(0.5) C22(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C30(H30A,H30B), C12(H12A,H12B), C37(H37A,H37B), C14(H14A,
 H14B), C28(H28A,H28B), C29(H29A,H29B), C15(H15A,H15B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C76(H76), C67(H67), C72(H72), C82(H82), C80(H80), C66(H66),
 C88(H88), C33(H33), C68(H68), C74(H74), C92(H92), C73(H73), C69(H69), C70(H70),
  C78(H78), C79(H79), C17(H17), C84(H84), C11(H11), C21(H21), C81(H81),
 C75(H75), C63(H63), C8(H8), C54(H54), C53(H53), C18(H18), C34(H34), C64(H64),
 C55(H55), C36(H36), C35(H35), C86(H86), C51(H51), C57(H57), C87(H87), C56(H56),
  C85(H85), C60(H60), C19(H19), C62(H62), C10(H10), C47(H47), C6(H6), C20(H20),
 C2(H2), C42(H42), C9(H9), C61(H61), C46(H46), C49(H49), C48(H48), C50(H50),
 C4(H4), C45(H45), C5(H5), C44(H44), C3(H3), C43(H43), C23(H23), C27A(H27A),
 C26A(H26A), C24(H24), C25A(H25A), C25(H25), C24A(H24A), C27(H27), C26(H26),
 C23A(H23A)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C89(H89C,H89B,H89A), C89(H89F,H89E,H89D)
;
_shelx_res_checksum              7858
_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 1.615
_oxdiff_exptl_absorpt_empirical_full_min 0.725