Self-assembled Co(II) and Co(III) [M<sub>2</sub>L<sub>3</sub>] helicates and [M<sub>4</sub>L<sub>6</sub>] tetrahedra from an unsymmetrical quaterpyridine ligand.
Siddique, Rashid G.; McMurtrie, John C.; Clegg, Jack K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11237–11241; doi:10.1039/d4dt01565g

data_7716401
_publ_section_title
;
 Self-assembled Co(II) and Co(III) [M<sub>2</sub>L<sub>3</sub>] helicates
 and [M<sub>4</sub>L<sub>6</sub>] tetrahedra from an unsymmetrical
 quaterpyridine ligand.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11237
_journal_page_last               11241
_journal_paper_doi               10.1039/d4dt01565g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C168 H108 Co4 N24, 2(Cl O4), 6[ClO4C2H3N]'
_chemical_formula_sum            'C168 H108 Cl2 Co4 N24 O8'
_chemical_formula_weight         2897.40
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                83.289(3)
_cell_angle_beta                 84.512(3)
_cell_angle_gamma                73.500(3)
_cell_formula_units_Z            2
_cell_length_a                   17.0436(6)
_cell_length_b                   22.9283(9)
_cell_length_c                   25.8861(10)
_cell_measurement_reflns_used    18360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3820
_cell_measurement_theta_min      1.9470
_cell_volume                     9612.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -18.00  77.00   1.00  110.00    --    2.42  57.00 -60.00   95
  2  \w     17.00  43.00   1.00  110.00    --   -3.98  77.00-180.00   26
  3  \w    -17.00  79.00   1.00  110.00    --    2.42  37.00-150.00   96
  4  \w    -24.00  70.00   1.00  110.00    --    2.42  77.00   0.00   94
  5  \w     23.00  48.00   1.00  110.00    --   -3.98  58.00 154.00   25
  6  \w    -35.00   8.00   1.00  110.00    --    2.42 -57.00 150.00   43
  7  \w    -29.00  10.00   1.00  110.00    --   -3.98 -58.00  14.00   39
  8  \w    -23.00  56.00   1.00  110.00    --   -3.98  57.00 120.00   79
  9  \w    -74.00 -37.00   1.00  110.00    --   -3.98 -58.00  14.00   37
 10  \w    -16.00  13.00   1.00  110.00    --   -3.98  77.00-180.00   29
 11  \w    -47.00 -18.00   1.00  110.00    --    2.42 -37.00-150.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0267339000
_diffrn_orient_matrix_UB_12      0.0298090000
_diffrn_orient_matrix_UB_13      0.0017183000
_diffrn_orient_matrix_UB_21      0.0240424000
_diffrn_orient_matrix_UB_22      0.0051192000
_diffrn_orient_matrix_UB_23      0.0190006000
_diffrn_orient_matrix_UB_31      0.0244803000
_diffrn_orient_matrix_UB_32      0.0116341000
_diffrn_orient_matrix_UB_33      -0.0200051000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            104725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.816
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.001
_exptl_crystal_description       plate
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         20090
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.1368
_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^)+(0.2000P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3637
_refine_ls_wR_factor_ref         0.3897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14687
_reflns_number_total             20090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01565g2.cif
_cod_data_source_block           sjkc19rr09
_cod_depositor_comments
'Adding full bibliography for 7716401--7716402.cif.'
_cod_original_cell_volume        9612.0(7)
_cod_database_code               7716401
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co4 C170 N12 H50 Cl8 O32'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C174-C173
 1.2 with sigma of 0.02
 C172-C173
 2.7 with sigma of 0.02
 C100-C101
 1.5 with sigma of 0.02
 C93-C96
 2.45 with sigma of 0.001
 C93-C100
 2.45 with sigma of 0.001
 C105-C98
 2.45 with sigma of 0.001
 C104-C98
 2.45 with sigma of 0.001
 C76-C72
 2.45 with sigma of 0.001
 C77-C72
 2.45 with sigma of 0.001
 C66-C67
 2.45 with sigma of 0.001
 C64-C67
 2.45 with sigma of 0.001
 Cl6-O1B \\sim Cl6-O1C \\sim Cl6-O1D \\sim Cl6-O1E
 with sigma of 0.02
 O1B-O1D \\sim O1C-O1E \\sim O1B-O1E \\sim O1C-O1D \\sim O1B-O1C \\sim O1D-O1E
 with sigma of 0.04
 C99-C102 \\sim C102-C178
 with sigma of 0.02
 C75-C73 \\sim C73-C69
 with sigma of 0.01
 C65-C74 \\sim C74-C68
 with sigma of 0.001
 C76-C72 \\sim C72-C77
 with sigma of 0.001
 C64-C67 \\sim C67-C66
 with sigma of 0.001
3. Restrained planarity
 C173, C174, C172, C171, C11, C14
 with sigma of 0.01
 C102, C101, C100, C99, C98, C97, C96, C178
 with sigma of 0.1
 C65, C67, C72, C75
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Cl6 \\sim O1B \\sim O1C \\sim O1D \\sim O1E: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C44) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43) =
Uanis(C46) = Uanis(C45)
Uiso(C13) = Uiso(C12) = Uiso(C16) = Uiso(C15) = Uiso(C17) = Uiso(C18)
Uanis(C152) = Uanis(C153) = Uanis(C156) = Uanis(C157) = Uanis(C158) =
Uanis(C151) = Uanis(C154) = Uanis(C155)
Uanis(C72) = Uanis(C69) = Uanis(C73) = Uanis(C74) = Uanis(C67) = Uanis(C68) =
Uanis(C70) = Uanis(C71)
Uanis(C98) = Uanis(C97) = Uanis(C96) = Uanis(C100) = Uanis(C101) = Uanis(C99)
Uiso(C17) = Uiso(C18) = Uiso(C15) = Uiso(C171) = Uiso(C172) = Uiso(C16) =
Uiso(C169) = Uiso(C12) = Uiso(C13)
Uiso(C174) = Uiso(C172)
Uanis(C71) = Uanis(C70) = Uanis(C69) = Uanis(C72) = Uanis(C73) = Uanis(C74) =
Uanis(C67) = Uanis(C68) = Uanis(C96) = Uanis(C97) = Uanis(C98) = Uanis(C99) =
Uanis(C178) = Uanis(C100) = Uanis(C101) = Uanis(C123) = Uanis(C130) =
Uanis(C129) = Uanis(C128) = Uanis(C124) = Uanis(C125) = Uanis(C126) =
Uanis(C127)
Uanis(C102) = Uanis(C101) = Uanis(C100) = Uanis(C99) = Uanis(C98) = Uanis(C97)
= Uanis(C96) = Uanis(C178)
5. Rigid body (RIGU) restrains
 Cl6, O1B, O1C, O1D, O1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, N18, C57, C58, C59, C60, C62, C63, C64, C65, C66, C75, C76, C77, C78,
 C79, N19, C80, C81, C82, C83, C84, N21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, C10, N24, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C100, C178, C96, C97, C98, C99, C127, C126, C125, C128, C129, C130,
 C123, C124
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C89, N20, C85, C86, C87, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C92, C93, C94, N22, C90, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C116, C117, N1, C113, C114, C115
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C16(0.5) H16(0.5) C15(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5)
 C17(0.5) C18(0.5) H18(0.5) C172(0.5) C171(0.5) H171(0.5) C169(0.5) H169(0.5)
 C170(0.5) H170(0.5) C174(0.5) C173(0.5) H173(0.5)
7.a Free rotating group:
 C39(C40,C41,C46,C45,C44,C42,C43), C129(C128,C125,C124,C123,C130,C126,C127),
 C11(C16,C15,C14,C13,C12,C17,C18), C157(C156,C153,C152,C151,C158,C154,C155),
 C67(C68,C69,C72,C73,C74,C70,C71), Cl6(O1B,O1C,O1D,O1E)
7.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C141(H141), C150(H150), C134(H134), C38(H38), C131(H131),
 C140(H140), C142(H142), C144(H144), C159(H159), C133(H133), C20(H20),
 C137(H137), C143(H143), C138(H138), C25(H25), C53(H53), C29(H29), C139(H139),
 C55(H55), C56(H56), C168(H168), C167(H167), C166(H166), C165(H165), C54(H54),
 C28(H28), C63(H63), C64(H64), C66(H66), C49(H49), C50(H50), C57(H57),
 C147(H147), C104(H104), C106(H106), C105(H105), C22(H22), C36(H36), C112(H112),
  C27(H27), C1(H1), C4(H4), C3(H3), C2(H2), C122(H122), C26(H26), C111(H111),
 C35(H35), C113(H113), C83(H83), C81(H81), C109(H109), C30(H30), C58(H58),
 C76(H76), C77(H77), C78(H78), C85(H85), C21(H21), C148(H148), C32(H32),
 C110(H110), C114(H114), C84(H84), C82(H82), C162(H162), C31(H31), C119(H119),
 C60(H60), C161(H161), C59(H59), C115(H115), C92(H92), C91(H91), C94(H94),
 C86(H86), C120(H120), C87(H87), C8(H8), C7(H7), C10(H10), C88(H88), C116(H116),
  C40(H40), C45(H45), C44(H44), C129(H129), C124(H124), C130(H130), C16(H16),
 C13(H13), C12(H12), C157(H157), C152(H152), C158(H158), C97(H97), C96(H96),
 C99(H99), C68(H68), C73(H73), C74(H74), C171(H171), C169(H169), C170(H170)
7.c Fitted hexagon refined as free rotating group:
 C164(N3,C168,C167,C166,C165), C62(C63,C64,C65,C66,N14), C104(N5,C107,C106,
 C105,C103), C1(N23,C5,C4,C3,C2), C79(N19,C76,C75,C77,C78), C92(C91,C90,N22,C94,
 C93), C8(C7,C6,N24,C10,C9), C97(C96,C178,C100,C99,C98)
7.d :
 C43(H43), C127(H127), C18(H18), C155(H155), C71(H71), C173(H173), C102(H102)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46924
_shelx_hkl_checksum              84512
_shelx_fab_checksum              7120
_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 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.630