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_7720673
_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         'C41 H46 N4 O2 P2 Zn, 2(C24 H20 B), C2 H3 N'
_chemical_formula_sum            'C91 H89 B2 N5 O2 P2 Zn'
_chemical_formula_weight         1433.60
_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'
_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                 106.049(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3820(2)
_cell_length_b                   35.6112(6)
_cell_length_c                   16.4596(3)
_cell_measurement_reflns_used    43951
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.6890
_cell_measurement_theta_min      1.7580
_cell_volume                     7538.1(2)
_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      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 0.896
_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      8.00  61.00   0.50    7.00    --   17.09-121.00 -63.00  106
  2  \w    -63.00 -14.00   0.50    7.00    --  -18.50 121.00  19.00   98
  3  \w    -62.00 -22.00   0.50    7.00    --   17.09 -19.00-150.00   80
  4  \w     -4.00  22.00   0.50    7.00    --   17.09  74.00-154.46   52
  5  \w     -3.00  28.00   0.50    7.00    --   17.09  72.00 -49.13   62
  6  \w      3.00  56.00   0.50    7.00    --   17.09  57.00-150.00  106
  7  \w    -62.00 -22.00   0.50    7.00    --   17.09 -19.00-180.00   80
  8  \w     -3.00  28.00   0.50    7.00    --   17.09  72.00 137.08   62
  9  \w     -3.00  28.00   0.50    7.00    --   17.09  72.00 -98.37   62
 10  \w      3.00  56.00   0.50    7.00    --   17.09  57.00 150.00  106
 11  \w    -62.00 -22.00   0.50    7.00    --   17.09 -19.00 -60.00   80
 12  \w    -62.00 -22.00   0.50    7.00    --   17.09 -19.00-120.00   80
 13  \w     18.00  60.00   0.50    7.00    --  -18.50  19.00  60.00   84
;
_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      -0.0084691000
_diffrn_orient_matrix_UB_12      -0.0183351000
_diffrn_orient_matrix_UB_13      0.0135850000
_diffrn_orient_matrix_UB_21      -0.0041802000
_diffrn_orient_matrix_UB_22      0.0074328000
_diffrn_orient_matrix_UB_23      0.0389020000
_diffrn_orient_matrix_UB_31      -0.0543443000
_diffrn_orient_matrix_UB_32      0.0022863000
_diffrn_orient_matrix_UB_33      -0.0176651000
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            124579
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.348
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63639
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.315
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         26172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0704P)^2^+5.8435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19575
_reflns_number_total             26172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_znbnnodpph_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720673
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn P N C B H O'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.959
_diffrn_oxdiff_ac3_digest_hkl    016913b022ba612bba46407213735e3f2bf052
_diffrn_oxdiff_digest_hkl
;
43d28175f29c856067dbd0d01f34731a97a22d
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C31(H31A,H31B), C29(H29A,H29B), C89(H89A,H89B), C14(H14A,
 H14B), C88(H88A,H88B), C15(H15A,H15B), C30(H30A,H30B), C16(H16A,H16B)
1.b Aromatic/amide H refined with riding coordinates:
 C57(H57), C41(H41), C43(H43), C51(H51), C49(H49), C33(H33), C53(H53),
 C12(H12), C44(H44), C45(H45), C50(H50), C28(H28), C11(H11), C48(H48), C47(H47),
  C42(H42), C34(H34), C59(H59), C54(H54), C72(H72), C71(H71), C63(H63),
 C55(H55), C56(H56), C35(H35), C8(H8), C69(H69), C73(H73), C37(H37), C24(H24),
 C10(H10), C75(H75), C68(H68), C74(H74), C27(H27), C36(H36), C2(H2), C60(H60),
 C9(H9), C6(H6), C62(H62), C61(H61), C67(H67), C26(H26), C18(H18), C25(H25),
 C65(H65), C66(H66), C77(H77), C87(H87), C83(H83), C81(H81), C19(H19), C22(H22),
  C20(H20), C3(H3), C86(H86), C5(H5), C80(H80), C85(H85), C4(H4), C84(H84),
 C79(H79), C78(H78), C21(H21)
1.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              94496
_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 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.703