Synthesis and characterization of heterometallic rings templated through alkylammonium or imidazolium cations.
Alotaibi, Rajeh; Booth, Amy; Little, Edmund; Brookfield, Adam; Achari, Amritroop; Lockyer, Selena J.; Timco, Grigore A.; Whitehead, George F. S.; Vitórica-Yrezábal, Iñigo J; Chilton, Nicholas F.; Nair, Rahul R.; Collison, David; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00982c

data_7713064
_publ_section_title
;
 Synthesis and characterization of heterometallic rings templated through
 alkylammonium or imidazolium cations.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00982c
_journal_year                    2023
_chemical_formula_moiety
'C85 H153 Cr8 F11 O34 Zn, 2(C3 H5 N2), [+ solvents]'
_chemical_formula_sum            'C93 H163 Cr8 F11 N2 O34 Zn'
_chemical_formula_weight         2543.61
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   36.4236(5)
_cell_length_b                   36.4236(5)
_cell_length_c                   19.1203(3)
_cell_measurement_reflns_used    14423
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.5790
_cell_measurement_theta_min      2.6870
_cell_volume                     21968.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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   -129.00 -20.00   1.00    1.00    --  -45.10 -34.00-117.00  109
  2  \w   -115.00 -47.00   1.00    5.00    -- -110.00  60.00  31.00   68
  3  \w   -184.00-123.00   1.00    5.00    -- -110.00 -60.00-108.00   61
  4  \w    -64.00   8.00   1.00    1.00    --  -45.10  60.00  31.00   72
  5  \w   -130.00 -21.00   1.00    5.00    -- -110.00  57.00-150.00  109
  6  \w   -150.00 -22.00   1.00    5.00    -- -110.00  38.00-150.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0371437000
_diffrn_orient_matrix_UB_12      -0.0271620000
_diffrn_orient_matrix_UB_13      0.0496210000
_diffrn_orient_matrix_UB_21      0.0288816000
_diffrn_orient_matrix_UB_22      0.0214635000
_diffrn_orient_matrix_UB_23      0.0635106000
_diffrn_orient_matrix_UB_31      -0.0128877000
_diffrn_orient_matrix_UB_32      0.0344066000
_diffrn_orient_matrix_UB_33      -0.0005218000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37098
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.227
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             7968
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         37098
_refine_ls_number_restraints     4069
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.2110
_refine_ls_R_factor_gt           0.1326
_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^)+(0.0826P)^2^+146.7259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2866
_refine_ls_wR_factor_ref         0.3416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20401
_reflns_number_total             37098
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 120.1670\% 
 around [-0.01 -0.05 1.00] (reciprocal) or [-0.01 -0.02 1.00] (direct)
;
_cod_data_source_file            d3dt00982c2.cif
_cod_data_source_block           s5330r_twin1_hklf4
_cod_original_cell_volume        21968.0(7)
_cod_database_code               7713064
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.218
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80933
 0.19067
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(Cr8) = Uanis(Cr7)
Uanis(F16A) = Uanis(F16)
Uanis(Zn12) = Uanis(Cr2)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Same fragment restrains
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, O4, C6, C7, C8, C9, C10}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, O6, C11, C12, C13, C14, C15}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, O8, C16, C17, C18, C19, C20}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, O10, C21, C22, C23, C24, C25}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, O12, C26, C27, C28, C29, C30}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13, O14, C31, C32, C33, C34, C35}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15, O16, C36, C37, C38, C39, C40}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1A, O2A, C1A, C2A, C3A, C4A, C5A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, O4A, C6A, C7A, C8A, C9A, C10A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, O6A, C11A, C12A, C13A, C14A, C15A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, O8A, C16A, C17A, C18A, C19A, C20A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, O10A, C21A, C22A, C23A, C24A, C25A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, O12A, C26A, C27A, C28A, C29A, C30A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13A, O14A, C31A, C32A, C33A, C34A, C35A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15A, O16A, C36A, C37A, C38A, C39A, C40A}
5. Others
 Fixed Sof: Cr6(0.5) F16(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C2H(0.5)
 H2HA(0.5) H2HB(0.5) H2HC(0.5) C1I(0.5) H1IA(0.5) H1IB(0.5) H1IC(0.5) Cr5(0.5)
 Cr8(0.5) Cr11(0.5) Zn12(0.5) F8(0.5) F10(0.5) F12(0.5) F13(0.5) O1(0.5)
 O2(0.5) C1(0.5) C2(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) O3(0.5) O4(0.5) C6(0.5)
 C7(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) O5(0.5) O6(0.5) C11(0.5) C12(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) O7(0.5) O8(0.5) C16(0.5) C17(0.5)
 C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
 C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) O9(0.5) O10(0.5) C21(0.5) C22(0.5)
 C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) O11(0.5) O12(0.5) C26(0.5) C27(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) O13(0.5) O14(0.5) C31(0.5) C32(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) O15(0.5) O16(0.5) C36(0.5) C37(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5)
 C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) Cr2(0.5) Cr7(0.5) Cr9(0.5) Cr10(0.5)
 F7(0.5) F9(0.5) F11(0.5) F15(0.5) O1A(0.5) O2A(0.5) C1A(0.5) C2A(0.5) C3A(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5A(0.5)
 H5AA(0.5) H5AB(0.5) H5AC(0.5) O3A(0.5) O4A(0.5) C6A(0.5) C7A(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C10A(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) O5A(0.5) O6A(0.5) C11A(0.5) C12A(0.5) C13A(0.5)
 H13D(0.5) H13E(0.5) H13F(0.5) C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
 C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5) O7A(0.5) O8A(0.5) C16A(0.5) C17A(0.5)
 C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19A(0.5) H19D(0.5) H19E(0.5)
 H19F(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5) O9A(0.5) O10A(0.5) C21A(0.5)
 C22A(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5)
 H24E(0.5) H24F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) O11A(0.5)
 O12A(0.5) C26A(0.5) C27A(0.5) C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5)
 C29A(0.5) H29D(0.5) H29E(0.5) H29F(0.5) C30A(0.5) H30D(0.5) H30E(0.5)
 H30F(0.5) O13A(0.5) O14A(0.5) C31A(0.5) C32A(0.5) C33A(0.5) H33D(0.5)
 H33E(0.5) H33F(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C35A(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5) O15A(0.5) O16A(0.5) C36A(0.5) C37A(0.5)
 C38A(0.5) H38D(0.5) H38E(0.5) H38F(0.5) C39A(0.5) H39D(0.5) H39E(0.5)
 H39F(0.5) C40A(0.5) H40D(0.5) H40E(0.5) H40F(0.5) F16A(0.5)
6.a Me refined with riding coordinates:
 C1B(H1BA,H1BB,H1BC), C2H(H2HA,H2HB,H2HC), C1I(H1IA,H1IB,H1IC), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C13A(H13D,H13E,
 H13F), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F), C25A(H25D,H25E,H25F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F),
 C30A(H30D,H30E,H30F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F), C35A(H35D,
 H35E,H35F), C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C41(H41), C51(H51), C3J(H3J), N2(H2)
;
_shelx_res_checksum              56611
_shelx_fab_checksum              24887
_platon_squeeze_special_details
;
A solvent mask was calculated and 826 electrons were 
found in a volume of 3508\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Asymmetric Unit 
which account for 720 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 2.035
_oxdiff_exptl_absorpt_empirical_full_min 0.579
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2