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_7720672
_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 N3 O3 P3 Zn, 2(C24 H20 B), C4 H10 O'
_chemical_formula_sum            'C97 H98 B2 N3 O4 P3 Zn'
_chemical_formula_weight         1549.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                118.0920(10)
_cell_angle_beta                 106.1320(10)
_cell_angle_gamma                97.1690(10)
_cell_formula_units_Z            2
_cell_length_a                   16.1174(2)
_cell_length_b                   18.4228(2)
_cell_length_c                   18.4245(2)
_cell_measurement_reflns_used    45185
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.9870
_cell_measurement_theta_min      2.2390
_cell_volume                     4420.25(11)
_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 0.884
_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    -60.00  23.00   0.50    3.58    --   13.07 -53.00-128.00  166
  2  \w    -60.00  23.00   0.50    3.58    --   13.07 -53.00-128.00  166
  3  \w      3.00  87.00   0.50    3.58    --   13.07  53.00  16.00  168
  4  \w      2.00  56.00   0.50    3.58    --   13.07  57.00 120.00  108
  5  \w    -65.00 -22.00   0.50    3.58    --   13.07 -19.00 150.00   86
  6  \w     -6.00  43.00   0.50    3.58    --   13.07 -99.00-120.00   98
  7  \w    -24.00  33.00   0.50    3.58    --   13.07 -77.00   0.00  114
  8  \w     -4.00  30.00   0.50    3.58    --   13.07  71.00  81.83   68
  9  \w     -6.00  43.00   0.50    3.58    --   13.07 -99.00 120.00   98
 10  \w     -4.00  30.00   0.50    3.58    --   13.07  71.00 172.59   68
 11  \w    -65.00 -22.00   0.50    3.58    --   13.07 -19.00 120.00   86
 12  \w    -48.00  -4.00   0.50    3.58    --  -14.48 105.00 136.90   88
 13  \w    -59.00 -17.00   0.50    3.58    --  -14.48 126.00  -8.39   84
 14  \w    -62.00  -3.00   0.50    3.58    --  -14.48 -57.00 150.00  118
 15  \w    -47.00  -3.00   0.50    3.58    --  -14.48 104.00  31.89   88
 16  \w    -42.00   5.00   0.50    3.58    --  -14.48  93.00-129.07   94
 17  \w    -88.00  -8.00   0.50    3.58    --  -14.48 -53.00-128.00  160
;
_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      -0.0232903000
_diffrn_orient_matrix_UB_12      -0.0161302000
_diffrn_orient_matrix_UB_13      -0.0458833000
_diffrn_orient_matrix_UB_21      -0.0303522000
_diffrn_orient_matrix_UB_22      0.0243054000
_diffrn_orient_matrix_UB_23      0.0105414000
_diffrn_orient_matrix_UB_31      0.0290709000
_diffrn_orient_matrix_UB_32      0.0352756000
_diffrn_orient_matrix_UB_33      0.0042956000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            132520
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.928
_diffrn_reflns_theta_min         2.174
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86766
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         29283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0592P)^2^+2.9307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22096
_reflns_number_total             29283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2024rk_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_original_cell_volume        4420.25(10)
_cod_database_code               7720672
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_ac3_digest_hkl    018b27d0c0d3a9d96dead362298a276e3c5d5f
_diffrn_oxdiff_digest_hkl
;
43cff372bc7ac76c9d11cdc8606b22ce806e89
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: O4(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5) C96(0.5) H96A(0.5)
 H96B(0.5) C94(0.5) H94A(0.5) H94B(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5)
 O5(0.5) C98(0.5) H98A(0.5) H98B(0.5) C100(0.5) H10A(0.5) H10B(0.5) C101(0.5)
 H10C(0.5) H10D(0.5) H10E(0.5) C99(0.5) H99A(0.5) H99B(0.5) H99C(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C14(H14A,H14B), C31(H31A,H31B), C15(H15A,
 H15B), C29(H29A,H29B), C45(H45A,H45B), C44(H44A,H44B), C30(H30A,H30B),
 C96(H96A,H96B), C94(H94A,H94B), C98(H98A,H98B), C100(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C87(H87), C86(H86), C65(H65), C85(H85), C89(H89), C79(H79), C78(H78),
 C22(H22), C80(H80), C66(H66), C83(H83), C84(H84), C24(H24), C63(H63), C62(H62),
  C93(H93), C6(H6), C53(H53), C8(H8), C12(H12), C90(H90), C18(H18), C73(H73),
 C2(H2), C4(H4), C5(H5), C28(H28), C21(H21), C61(H61), C91(H91), C3(H3),
 C92(H92), C19(H19), C9(H9), C43(H43), C20(H20), C67(H67), C10(H10), C68(H68),
 C54(H54), C75(H75), C72(H72), C69(H69), C59(H59), C51(H51), C33(H33), C11(H11),
  C25(H25), C60(H60), C57(H57), C47(H47), C55(H55), C56(H56), C39(H39),
 C27(H27), C37(H37), C70(H70), C34(H34), C71(H71), C26(H26), C50(H50), C42(H42),
  C35(H35), C48(H48), C49(H49), C36(H36), C41(H41), C40(H40)
2.c Idealised Me refined as rotating group:
 C97(H97A,H97B,H97C), C95(H95A,H95B,H95C), C101(H10C,H10D,H10E), C99(H99A,H99B,
 H99C)
;
_shelx_res_checksum              20801
_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 2.520
_oxdiff_exptl_absorpt_empirical_full_min 0.636