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_7720666
_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 Ni O2 P2, 2(C24 H20 B), C2 H3 N'
_chemical_formula_sum            'C91 H89 B2 N5 Ni O2 P2'
_chemical_formula_weight         1426.94
_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                 106.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5349(2)
_cell_length_b                   35.3829(7)
_cell_length_c                   16.3968(3)
_cell_measurement_reflns_used    37470
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.5520
_cell_measurement_theta_min      1.8130
_cell_volume                     7547.5(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 0.903
_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      3.00  57.00   0.50    6.28    --   17.09-113.00  78.00  108
  2  \w    -58.00  -9.00   0.50    6.28    --  -18.50 113.00 170.00   98
  3  \w    -62.00 -22.00   0.50    6.28    --   17.09 -19.00-150.00   80
  4  \w      3.00  56.00   0.50    6.28    --   17.09  57.00-150.00  106
  5  \w    -62.00 -22.00   0.50    6.28    --   17.09 -19.00   0.00   80
  6  \w      3.00  56.00   0.50    6.28    --   17.09  57.00 150.00  106
  7  \w      3.00  56.00   0.50    6.28    --   17.09  57.00 -60.00  106
  8  \w     16.00  62.00   0.50    6.28    --  -18.50  19.00-120.00   92
  9  \w    -62.00  -4.00   0.50    6.28    --  -18.50 -57.00  60.00  116
 10  \w     16.00  62.00   0.50    6.28    --  -18.50  19.00 120.00   92
 11  \w      3.00  38.00   0.50    6.28    --   17.09  57.00  30.00   70
;
_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      -0.0058721000
_diffrn_orient_matrix_UB_12      -0.0111891000
_diffrn_orient_matrix_UB_13      -0.0369331000
_diffrn_orient_matrix_UB_21      0.0081294000
_diffrn_orient_matrix_UB_22      0.0162234000
_diffrn_orient_matrix_UB_23      -0.0227269000
_diffrn_orient_matrix_UB_31      0.0535899000
_diffrn_orient_matrix_UB_32      -0.0036750000
_diffrn_orient_matrix_UB_33      0.0120313000
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            124747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.375
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34997
_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    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         26475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+4.0862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19171
_reflns_number_total             26475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00255b2.cif
_cod_data_source_block           2025rk_nibnnodpph_auto
_cod_depositor_comments
'Adding full bibliography for 7720665--7720675.cif.'
_cod_database_code               7720666
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni B P O C H N'
_diffrn_oxdiff_ac3_digest_hkl    014f8bfd6077e0b1c6c670aaa14cb2fa8154dd
_diffrn_oxdiff_digest_hkl
;
4350b568bc6cf6f5f8fb6ed1bad4b49720a770
;
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C13(H13A,H13B), C29(H29A,H29B), C14(H14A,H14B), C38(H38A,
 H38B), C16(H16A,H16B), C30(H30A,H30B), C15(H15A,H15B), C37(H37A,H37B)
1.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C53(H53), C61(H61), C43(H43), C55(H55), C45(H45), C64(H64),
 C51(H51), C63(H63), C62(H62), C24(H24), C12(H12), C49(H49), C50(H50), C59(H59),
  C32(H32), C91(H91), C46(H46), C52(H52), C33(H33), C11(H11), C72(H72),
 C44(H44), C74(H74), C87(H87), C78(H78), C8(H8), C76(H76), C75(H75), C88(H88),
 C58(H58), C36(H36), C28(H28), C34(H34), C25(H25), C84(H84), C86(H86), C2(H2),
 C56(H56), C35(H35), C57(H57), C10(H10), C73(H73), C66(H66), C22(H22), C26(H26),
  C82(H82), C70(H70), C85(H85), C80(H80), C27(H27), C6(H6), C79(H79), C18(H18),
 C3(H3), C81(H81), C69(H69), C9(H9), C21(H21), C4(H4), C68(H68), C67(H67),
 C20(H20), C19(H19), C5(H5)
1.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              3272
_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 1.785
_oxdiff_exptl_absorpt_empirical_full_min 0.513