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_7716402
_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, 7(F6 P), 5[PF6C6H9N3]'
_chemical_formula_sum            'C198 H153 Co4 F72 N39 P12'
_chemical_formula_weight         5053.95
_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             2024-05-27
_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                97.0320(10)
_cell_angle_beta                 98.7350(10)
_cell_angle_gamma                119.772(2)
_cell_formula_units_Z            2
_cell_length_a                   21.0998(4)
_cell_length_b                   21.1425(4)
_cell_length_c                   34.7365(5)
_cell_measurement_reflns_used    55100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2300
_cell_measurement_theta_min      1.9620
_cell_volume                     12936.4(5)
_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 2014/5 (Sheldrick, 2014)'
_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 0.946
_diffrn_measured_fraction_theta_max 0.946
_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   0.50  130.00    --    2.42  57.00 -30.00  190
  2  \w      4.00  41.00   0.50  130.00    --    2.42  57.00-120.00   74
  3  \w    -63.00   6.00   0.50  130.00    --   -3.82 -37.00-150.00  138
  4  \w    -68.00  23.00   0.50  130.00    --   -3.82 -77.00  30.00  182
;
_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      0.0158317000
_diffrn_orient_matrix_UB_12      -0.0137123000
_diffrn_orient_matrix_UB_13      -0.0128124000
_diffrn_orient_matrix_UB_21      -0.0131121000
_diffrn_orient_matrix_UB_22      0.0120905000
_diffrn_orient_matrix_UB_23      -0.0158472000
_diffrn_orient_matrix_UB_31      0.0342798000
_diffrn_orient_matrix_UB_32      0.0352692000
_diffrn_orient_matrix_UB_33      0.0059675000
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            109822
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.220
_diffrn_reflns_theta_max         25.220
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38699
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       plate
_exptl_crystal_F_000             5100
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.492
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1999
_refine_ls_number_reflns         44190
_refine_ls_number_restraints     2295
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.1201
_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^)+(0.1000P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29598
_reflns_number_total             44190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01565g2.cif
_cod_data_source_block           sjkc19rr10
_cod_depositor_comments
'Adding full bibliography for 7716401--7716402.cif.'
_cod_database_code               7716402
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co4 C160 N24 P12 F72 H30'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 94.75
_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. Uiso/Uaniso restraints and constraints
Uanis(C71) = Uanis(C72) = Uanis(C67) = Uanis(C68) = Uanis(C69) = Uanis(C70) =
Uanis(C73) = Uanis(C74)
Uanis(C41) = Uanis(C39) = Uanis(C40) = Uanis(C46) = Uanis(C45) = Uanis(C42) =
Uanis(C43) = Uanis(C44)
Uanis(C158) = Uanis(C157) = Uanis(C156) = Uanis(C155) = Uanis(C154) =
Uanis(C153) = Uanis(C152) = Uanis(C151)
3. Rigid body (RIGU) restrains
 C95, C96, C97, C98, C99, C100, C101, C102
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C127, C128, C123, C124, C125, C126, C129, C130
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 N1, C56, C55, C54, C53, C52
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 C154(C155,C156,C151,C152,C153,C157,C158), C69(C70,C71,C72,C67,C68,C73,C74),
 C46(C45,C42,C41,C39,C40,C43,C44), P4(F3,F4,F5,F6,F7,F2)
4.b Aromatic/amide H refined with riding coordinates:
 C94(H94), C132(H132), C1(H1), C10(H10), C87(H87), C104(H104), C85(H85),
 C38(H38), C86(H86), C88(H88), C2(H2), C140(H140), C150(H150), C20(H20),
 C91(H91), C76(H76), C92(H92), C22(H22), C137(H137), C4(H4), C82(H82), C84(H84),
  C21(H21), C28(H28), C25(H25), C109(H109), C139(H139), C116(H116), C122(H122),
 C111(H111), C83(H83), C8(H8), C56(H56), C55(H55), C54(H54), C53(H53), C3(H3),
 C81(H81), C106(H106), C112(H112), C48(H48), C29(H29), C113(H113), C110(H110),
 C66(H66), C138(H138), C30(H30), C7(H7), C26(H26), C144(H144), C115(H115),
 C114(H114), C27(H27), C143(H143), C18(H18), C105(H105), C134(H134), C119(H119),
  C120(H120), C160(H160), C32(H32), C141(H141), C142(H142), C31(H31),
 C133(H133), C147(H147), C35(H35), C17(H17), C36(H36), C168(H168), C148(H148),
 C96(H96), C167(H167), C60(H60), C97(H97), C57(H57), C64(H64), C127(H127),
 C77(H77), C49(H49), C12(H12), C59(H59), C99(H99), C125(H125), C63(H63),
 C78(H78), C161(H161), C166(H166), C50(H50), C162(H162), C165(H165), C58(H58),
 C155(H155), C152(H152), C153(H153), C69(H69), C72(H72), C68(H68), C46(H46),
 C41(H41), C40(H40), C124(H124)
4.c Fitted hexagon refined as free rotating group:
 N1(C56,C55,C54,C53,C52)
4.d :
 C15(H15), C130(H130), C102(H102), C158(H158), C74(H74), C44(H44)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30870
_shelx_hkl_checksum              49159
_shelx_fab_checksum              16029
_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 3.747
_oxdiff_exptl_absorpt_empirical_full_min 0.611