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_7720675
_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 N4 O3 P3 Zn, 2(N O3), 6[C2H3N]'
_chemical_formula_sum            'C66 H77 N12 O9 P3 Zn'
_chemical_formula_weight         1340.739
_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             2025-12-14
_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                 90.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9010(2)
_cell_length_b                   19.0309(3)
_cell_length_c                   24.1395(4)
_cell_measurement_reflns_used    23367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4870
_cell_measurement_theta_min      2.5340
_cell_volume                     5926.24(16)
_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 0.9835
_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    -39.00  31.00   0.50    8.24    --   11.06 -69.00 -42.00  140
  2  \w    -39.00   7.00   0.50    8.24    --  -12.47 -69.00 -42.00   92
  3  \w    -32.00  33.00   0.50    8.24    --  -12.47  69.00  89.00  130
  4  \w    -70.00 -22.00   0.50    8.24    --   11.06 -19.00  90.00   96
  5  \w    -35.00  18.00   0.50    8.24    --  -12.47  77.00 120.00  106
  6  \w     16.00  68.00   0.50    8.24    --  -12.47  19.00  30.00  104
  7  \w     16.00  68.00   0.50    8.24    --  -12.47  19.00-120.00  104
  8  \w    -35.00  14.00   0.50    8.24    --  -12.47  77.00-180.00   98
;
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9835
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            74586
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9835
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68753
_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    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             2820.284
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of MeCN and Et2O  by slow evaporation'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.3139
_refine_diff_density_min         -0.8289
_refine_diff_density_rms         0.1310
_refine_ls_d_res_high            0.7448
_refine_ls_d_res_low             9.8017
_refine_ls_goodness_of_fit_ref   1.0438
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    106
_refine_ls_number_parameters     658
_refine_ls_number_reflns         14769
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.0415
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+12.9725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1714
_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                11485
_reflns_number_total             14769
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_ZnbnDOTPphNO3_autored
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_original_formula_sum        'C66 H77 N12 O9 P3 Zn1'
_cod_database_code               7720675
_chemical_oxdiff_formula         'Zn N O P C H '
_chemical_oxdiff_usercomment     'CSD: NOLQEK'
_cell_oxdiff_angle_alpha         90.0157(12)
_cell_oxdiff_angle_beta          90.7037(12)
_cell_oxdiff_angle_gamma         89.9788(11)
_cell_oxdiff_length_a            12.90174(18)
_cell_oxdiff_length_b            19.0302(3)
_cell_oxdiff_length_c            24.1390(4)
_cell_oxdiff_measurement_reflns_used 23367
_cell_oxdiff_volume              5926.22(15)
_diffrn_oxdiff_measurement_exp_name 2025rk_ZnbnDOTPphNO3.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O6 \\sim N5: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O6) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
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.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)
5.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),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
;
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.747