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_7720665
_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 Cu N3 O3 P3, Cu N4 O12'
_chemical_formula_sum            'C45 H48 Cu2 N7 O15 P3'
_chemical_formula_weight         1146.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 96.213(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1326(2)
_cell_length_b                   20.3581(3)
_cell_length_c                   19.3113(4)
_cell_measurement_reflns_used    14641
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.5100
_cell_measurement_theta_min      2.3210
_cell_volume                     4741.81(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.863
_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      2.00  95.00   0.50   18.30    --   15.30  32.00 -73.00  186
  2  \w    -63.00   6.00   0.50   18.30    --   15.30 -32.00 127.00  138
  3  \w    -63.00 -24.00   0.50   18.30    --   15.30 -19.00   0.00   78
  4  \w     19.00  53.00   0.50   18.30    --   15.30  57.00 -30.00   68
  5  \w      7.00  48.00   0.50   18.30    --   15.30 -99.00  30.00   82
  6  \w     13.00  39.00   0.50   18.30    --   15.30  57.00  60.00   52
;
_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      0.0181447000
_diffrn_orient_matrix_UB_12      -0.0128874000
_diffrn_orient_matrix_UB_13      -0.0309628000
_diffrn_orient_matrix_UB_21      0.0534258000
_diffrn_orient_matrix_UB_22      -0.0054950000
_diffrn_orient_matrix_UB_23      0.0178360000
_diffrn_orient_matrix_UB_31      -0.0165493000
_diffrn_orient_matrix_UB_32      -0.0318998000
_diffrn_orient_matrix_UB_33      0.0094160000
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.570
_diffrn_reflns_theta_min         1.894
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62291
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.357
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         14892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0604P)^2^+10.7515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11358
_reflns_number_total             14892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2024rk_ks_cunotpph_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720665
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O P H Cu'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.928
_diffrn_oxdiff_ac3_digest_hkl    01d30b196cd85a2231a0e03f0efa34ee7c642b
_diffrn_oxdiff_digest_hkl
;
438d62c931d26d3ef72ba87f34d1bb7451e5bd
;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C29(H29A,H29B), C14(H14A,H14B), C15(H15A,
 H15B), C45(H45A,H45B), C44(H44A,H44B), C16(H16A,H16B), C13(H13A,H13B)
1.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C22(H22), C6(H6), C5(H5), C39(H39), C2(H2), C4(H4), C24(H24),
 C34(H34), C43(H43), C28(H28), C18(H18), C26(H26), C42(H42), C37(H37), C21(H21),
  C3(H3), C35(H35), C27(H27), C33(H33), C10(H10), C41(H41), C12(H12), C36(H36),
 C19(H19), C9(H9), C11(H11), C8(H8), C20(H20), C40(H40)
;
_shelx_res_checksum              81845
_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 2.066
_oxdiff_exptl_absorpt_empirical_full_min 0.658