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_7720670
_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         'C39 H43 Cu2 N7 O14 P2'
_chemical_formula_sum            'C39 H43 Cu2 N7 O14 P2'
_chemical_formula_weight         1022.82
_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                 94.3010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.01010(10)
_cell_length_b                   17.9328(2)
_cell_length_c                   24.3639(3)
_cell_measurement_reflns_used    37949
_cell_measurement_temperature    99.9(9)
_cell_measurement_theta_max      33.5440
_cell_measurement_theta_min      2.0290
_cell_volume                     4361.23(8)
_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      99.9(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_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    -36.00  37.00   0.50    1.00    --   17.09 -71.00 124.00  146
  2  \w    -62.00 -22.00   0.50    1.00    --   17.09 -19.00   0.00   80
  3  \w    -62.00 -22.00   0.50    1.00    --   17.09 -19.00 -30.00   80
  4  \w      3.00  56.00   0.50    1.00    --   17.09  57.00-120.00  106
  5  \w      3.00  56.00   0.50    1.00    --   17.09  57.00 -30.00  106
  6  \w      3.00  34.00   0.50    1.00    --   17.09  57.00  60.00   62
  7  \w    -41.00  18.00   0.50    1.00    --  -18.50  77.00 -30.00  118
  8  \w    -39.00  30.00   0.50    1.00    --  -18.50  71.00-104.00  138
  9  \w     16.00  62.00   0.50    1.00    --  -18.50  19.00-180.00   92
 10  \w    -62.00  -4.00   0.50    1.00    --  -18.50 -57.00  60.00  116
;
_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      -0.0193402000
_diffrn_orient_matrix_UB_12      -0.0310996000
_diffrn_orient_matrix_UB_13      0.0155554000
_diffrn_orient_matrix_UB_21      -0.0566815000
_diffrn_orient_matrix_UB_22      -0.0055235000
_diffrn_orient_matrix_UB_23      -0.0188314000
_diffrn_orient_matrix_UB_31      0.0383540000
_diffrn_orient_matrix_UB_32      -0.0238070000
_diffrn_orient_matrix_UB_33      -0.0159451000
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            71809
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.420
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78712
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         15301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0419P)^2^+1.9416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12481
_reflns_number_total             15301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_cubnnodpphmecn_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu N O P C H'
_chemical_oxdiff_usercomment     'CSD: YOHBOO'
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.886
_diffrn_oxdiff_ac3_digest_hkl    0109f8983bc123f0b08dac23132f39c5d6622e
_diffrn_oxdiff_digest_hkl
;
4387229ed26704889583dcb9ed47c83f7033bd
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C38(H38A,H38B), C39(H39A,H39B), C14(H14A,H14B), C23(H23A,
 H23B), C15(H15A,H15B), C25(H25A,H25B), C16(H16A,H16B), C24(H24A,H24B)
1.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C33(H33), C5(H5), C37(H37), C1(H1), C12(H12), C19(H19), C11(H11),
 C31(H31), C2(H2), C4(H4), C34(H34), C20(H20), C29(H29), C27(H27), C36(H36),
 C30(H30), C22(H22), C10(H10), C35(H35), C3(H3), C8(H8), C21(H21), C28(H28),
 C9(H9)
;
_shelx_res_checksum              79345
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.829