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_7720669
_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 Co N4 O3 P3, 2(N O3), 2[C4H10O]'
_chemical_formula_sum            'C62 H79 Co N6 O11 P3'
_chemical_formula_weight         1236.207
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-15 deposited with the CCDC.	2026-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.483(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9014(3)
_cell_length_b                   19.0597(3)
_cell_length_c                   24.0169(5)
_cell_measurement_reflns_used    22144
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8600
_cell_measurement_theta_min      2.2910
_cell_volume                     5905.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.44.118a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.94a 64-bit (release 17-02-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.118a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9874
_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    -14.00  66.00   0.50   60.00    --  -12.47  33.00 -93.00  160
  2  \w    -91.00   2.00   0.50   60.00    --  -12.47 -33.00 108.00  186
  3  \w     -6.00  44.00   0.50   60.00    --   11.06 -99.00  30.00  100
  4  \w     -6.00  44.00   0.50   60.00    --   11.06 -99.00 -60.00  100
  5  \w     -6.00  44.00   0.50   60.00    --   11.06 -99.00  90.00  100
  6  \w    -70.00 -22.00   0.50   60.00    --   11.06 -19.00  30.00   96
  7  \w    -35.00  18.00   0.50   60.00    --  -12.47  77.00 -60.00  106
  8  \w     16.00  41.00   0.50   60.00    --   11.06  19.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9874
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75995
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9874
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.118a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       needle
_exptl_crystal_F_000             2616.268
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of MeCN and methanol  by slow evaporation'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.8624
_refine_diff_density_min         -0.8761
_refine_diff_density_rms         0.1612
_refine_ls_d_res_high            0.7448
_refine_ls_d_res_low             10.1598
_refine_ls_goodness_of_fit_ref   1.0468
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    121
_refine_ls_number_parameters     665
_refine_ls_number_reflns         14779
_refine_ls_number_restraints     773
_refine_ls_restrained_S_all      1.0193
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+25.0956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2546
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                10890
_reflns_number_total             14779
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_Cobndotpphno3_autored
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_original_formula_sum        'C62 H79 Co1 N6 O11 P3'
_cod_database_code               7720669
_chemical_oxdiff_formula         'Co N P O C H'
_chemical_oxdiff_usercomment     'CSD: NOLQEK'
_cell_oxdiff_angle_alpha         90.058(2)
_cell_oxdiff_angle_beta          90.453(2)
_cell_oxdiff_angle_gamma         89.9940(17)
_cell_oxdiff_length_a            12.9015(3)
_cell_oxdiff_length_b            19.0626(4)
_cell_oxdiff_length_c            24.0129(7)
_cell_oxdiff_measurement_reflns_used 22144
_cell_oxdiff_volume              5905.5(2)
_diffrn_oxdiff_measurement_exp_name 2025rk_Cobndotpphno3.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P3-C29A \\sim P3-C29B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30A \\sim C30B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C43) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C29B)=Sof(C34B)=Sof(H34B)=Sof(C33B)=Sof(H33B)=Sof(C32B)=Sof(H32B)=
 Sof(C31B)=Sof(H31B)=Sof(C30B)=Sof(H30B)=1-FVAR(1)
 Sof(C29A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=
 Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C22(H22a,H22b), C35(H35a,H35b),
 C42(H42a,H42b)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C54(H54), C53(H53), C52(H52), C51(H51), C50(H50),
  C34A(H34A), C33A(H33A), C32A(H32A), C31A(H31A), C30A(H30A), C34B(H34B),
 C33B(H33B), C32B(H32B), C31B(H31B), C30B(H30B)
6.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C49(C54,C53,C52,C51,C50), C29A(C34A,C33A,C32A,C31A,
 C30A), C29B(C34B,C33B,C32B,C31B,C30B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.660