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_7713059
_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
'C91.903 H165.425 Cr8 F12 O36.761 Zn2, C10 H18 N4, 2.643(C4 H8 O), 2(C0.64 H1.921 N0.32)'
_chemical_formula_sum            'C113.68 H208.26 Cr8 F12 N4.64 O39.38 Zn2'
_chemical_formula_weight         3045.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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                90
_cell_formula_units_Z            4
_cell_length_a                   33.2596(4)
_cell_length_b                   20.8631(3)
_cell_length_c                   22.6682(3)
_cell_measurement_reflns_used    11373
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.2590
_cell_measurement_theta_min      4.2320
_cell_volume                     15729.4(4)
_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 2019/3 (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 0.996
_diffrn_measured_fraction_theta_max 0.973
_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    -28.00  -2.00   1.00    1.00    --    5.00 -26.00 -64.00   26
  2  \w    -54.00 -29.00   1.00    1.00    --  -45.10  26.00  98.00   25
  3  \w   -131.00 -83.00   1.00    1.00    --  -45.10 -26.00 -64.00   48
  4  \w    -76.00 -51.00   1.00    4.00    -- -110.00  26.00  98.00   25
  5  \w   -162.00 -57.00   1.00    4.00    -- -110.00 -26.00 -64.00  105
  6  \w   -131.00 -12.00   1.00    1.00    --  -45.10 -57.00-150.00  119
  7  \w    -76.00 -50.00   1.00    4.00    -- -110.00  57.00  30.00   26
  8  \w   -151.00 -22.00   1.00    4.00    -- -110.00  38.00 -60.00  129
  9  \w   -123.00 -54.00   1.00    4.00    -- -110.00  76.00-120.00   69
 10  \w    -48.00 -22.00   1.00    4.00    -- -110.00  57.00 -60.00   26
 11  \w   -113.00 -64.00   1.00    4.00    -- -110.00  57.00 -60.00   49
;
_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      0.0152418000
_diffrn_orient_matrix_UB_12      0.0146944000
_diffrn_orient_matrix_UB_13      -0.0626648000
_diffrn_orient_matrix_UB_21      0.0043742000
_diffrn_orient_matrix_UB_22      -0.0723649000
_diffrn_orient_matrix_UB_23      -0.0120936000
_diffrn_orient_matrix_UB_31      -0.0435320000
_diffrn_orient_matrix_UB_32      -0.0021106000
_diffrn_orient_matrix_UB_33      -0.0232306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31103
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.133
_diffrn_reflns_theta_min         4.238
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80312
_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    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             6391
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         8250
_refine_ls_number_restraints     2215
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0490
_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^)+(0.1016P)^2^+5.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6321
_reflns_number_total             8250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00982c2.cif
_cod_data_source_block           s5332r
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7713059
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.581
_shelx_estimated_absorpt_t_min   0.265
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Shared sites
{Cr1, Zn1}
{Cr1A, Zn1A}
2. Restrained distances
 C48-C47
 1.54 with sigma of 0.02
 C49-C47 = C48_$1-C47 = C24A-C47 = C48-C47
 1.54 with sigma of 0.02
 C20-C17 = C18-C17 = C19-C17
 1.54 with sigma of 0.02
 C1H-C1G = C1G-C1F = C1F-C1E = C1D-C1C = C1C-C1B = C1B-C1A
 1.54 with sigma of 0.02
 O18-C1E = O18-C1H = O19-C1D = O19-C1A
 1.35 with sigma of 0.02
 C50-C46
 1.45 with sigma of 0.02
 N4-C50
 1.14 with sigma of 0.02
 C64-C63_$1 \\sim C63_$1-C63
 with sigma of 0.02
 C1F-C1H \\sim C1E-C1G
 with sigma of 0.04
 O18-C1F \\sim O18-C1G
 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O19-C1B \\sim O19-C1C
 with sigma of 0.04
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 C1E-C1F \\sim C1F-C1G \\sim C1G-C1H
 with sigma of 0.02
 O19-C1A \\sim O19-C1D
 with sigma of 0.02
 O18-C1E \\sim O18-C1H
 with sigma of 0.02
 C1H-C1E \\sim C1D-C1A
 with sigma of 0.02
 C1G-C1E \\sim C1H-C1F \\sim C1C-C1A \\sim C1D-C1B
 with sigma of 0.02
 O19-C1C \\sim O19-C1B \\sim O18-C1F \\sim O18-C1G
 with sigma of 0.02
 Cr1A-F8 \\sim Zn1A-F8 \\sim Zn1-F1 \\sim Cr1-F1
 with sigma of 0.02
 Zn1-F2 \\sim Cr1-F2 \\sim Cr1A-F9 \\sim Zn1A-F9
 with sigma of 0.02
3. Restrained planarity
 O20, C61, O20_$1, C62
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(Cr1A) = Uanis(Zn1A)
Uanis(Cr1) = Uanis(Zn1)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. 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
{O8, O21, C16, C17, C18, C19, C20}
{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
{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
{O10, O9, 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}
{C1, C2, C3, C4} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C61, C62, C63, C64}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O14, O13, C31, C32, C33, C34, C35}
7. Others
 Sof(C46)=Sof(C50)=Sof(N4)=0.5*FVAR(2)
 Sof(O19)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 FVAR(1)
 Sof(O18)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=
 Sof(H1GA)=Sof(H1GB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=FVAR(2)
 Sof(O20)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=1-FVAR(3)
 Sof(F7)=Sof(C61)=Sof(C62)=Sof(C64)=Sof(H64C)=Sof(H64B)=Sof(H64A)=Sof(Cr1A)=
 Sof(Zn1A)=0.5*(1-FVAR(4))
 Sof(F8)=Sof(F9)=0.25*(1-FVAR(4))
 Sof(Zn1)=Sof(Cr1)=Sof(F1)=Sof(F2)=0.5*FVAR(4)
 Fixed Sof: Cr3(0.5) C47(0.25) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C49(0.5)
 H49A(0.5) H49B(0.5) H49C(0.5) C24A(0.5) H24A(0.5) H24B(0.5) H24C(0.5) N1(0.5)
 H1(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) C44(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) Cr2(0.5) F3(0.5)
 F4(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) O8(0.5) O21(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) O14(0.5) O13(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) Cr4(0.5) F6(0.5)
 F5(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) O10(0.5) O9(0.5) C21(0.5) C22(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C24(0.5) H24D(0.5) H24E(0.5) H24F(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)
8.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,
 H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB)
8.b Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C24A(H24A,H24B,H24C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), 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), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C23(H23A,H23B,H23C), C24(H24D,H24E,H24F), C25(H25A,H25B,H25C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C63(H63A,H63B,H63C), C64(H64C,
 H64B,H64A)
8.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C41(H41), C42(H42)
8.d Idealised Me refined with riding coordinates:
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              86224
_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 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.760