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_7713062
_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
'C80 H144 Cr6 F8 O32 Zn2, 2(C3 H5 N2), 0.5(C7 H8)'
_chemical_formula_sum            'C89.5 H158 Cr6 F8 N4 O32 Zn2'
_chemical_formula_weight         2396.93
_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             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                 111.085(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1079(6)
_cell_length_b                   16.8130(3)
_cell_length_c                   31.3860(8)
_cell_measurement_reflns_used    17988
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.8630
_cell_measurement_theta_min      1.5050
_cell_volume                     12362.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.863
_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     14.00 105.00   1.00    2.00    --   20.00  50.00   0.00   91
  2  \w    -69.00  60.00   1.00    2.00    --   20.00  60.00 120.00  129
  3  \w     71.00 108.00   1.00    2.00    --   20.00  60.00 120.00   37
  4  \w    -68.00 -43.00   1.00    2.00    --   20.00  50.00  30.00   25
  5  \w     80.00 106.00   1.00    2.00    --   20.00  50.00  30.00   26
  6  \w    -69.00 -28.00   1.00    2.00    --   20.00  50.00   0.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027052000
_diffrn_orient_matrix_UB_12      -0.0304275000
_diffrn_orient_matrix_UB_13      -0.0147574000
_diffrn_orient_matrix_UB_21      -0.0077268000
_diffrn_orient_matrix_UB_22      -0.0288290000
_diffrn_orient_matrix_UB_23      0.0132238000
_diffrn_orient_matrix_UB_31      -0.0291422000
_diffrn_orient_matrix_UB_32      0.0048229000
_diffrn_orient_matrix_UB_33      -0.0139410000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            74940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.093
_diffrn_reflns_theta_min         1.491
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             5020
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1670
_refine_ls_number_reflns         28605
_refine_ls_number_restraints     2438
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+8.4217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18403
_reflns_number_total             28605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00982c2.cif
_cod_data_source_block           s5268l
_cod_original_formula_sum        'C89.50 H158 Cr6 F8 N4 O32 Zn2'
_cod_database_code               7713062
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Cr8F8O32C100H100
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.861
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{Cr1, Zn1}
{Cr2, Zn2}
{Cr3, Zn3}
{Cr4, Zn4}
{Cr5, Zn5}
{Cr6, Zn6}
{Cr7, Zn7}
{Cr8, Zn8}
2. Restrained distances
 N57-C38
 2.1 with sigma of 0.02
 C7-C42 \\sim C7-C42A
 with sigma of 0.02
 N57A-C45A \\sim N57A-C32A \\sim N57-C45 \\sim N57-C32 \\sim N37-C38 \\sim
N37-C32 \\sim N37A-C38A ~
 N37A-C32A \\sim N31A-C22A \\sim N31-C22 \\sim N31A-C43A \\sim N31-C43 \\sim
N1A-C34A \\sim N1-C34 ~
 N1A-C22A \\sim N1-C22
 with sigma of 0.02
 C42-C81 \\sim C42A-C81A
 with sigma of 0.02
 C45-C38 \\sim C45A-C38A \\sim C43A-C34A \\sim C43-C34
 with sigma of 0.02
 C43A-C22A \\sim C43-C22 \\sim C34A-C22A \\sim C34-C22 \\sim C38-C32 \\sim
C38A-C32A \\sim C45-C32 ~
 C45A-C32A
 with sigma of 0.04
 N31-N1 \\sim N31A-N1A \\sim N57-N37 \\sim N57A-N37A
 with sigma of 0.04
 C16-C67 \\sim C16-C67A
 with sigma of 0.04
 C42-C87 \\sim C42A-C87A
 with sigma of 0.02
 C42-C94 \\sim C42A-C94A
 with sigma of 0.02
 C48-C69 \\sim C48A-C69A
 with sigma of 0.02
 C7-C81 \\sim C7-C81A
 with sigma of 0.04
 C13-C36 \\sim C13-C36A
 with sigma of 0.02
 C7-C87 \\sim C7-C87A
 with sigma of 0.04
 C13-C83 \\sim C13-C83A
 with sigma of 0.04
 C7-C94 \\sim C7-C94A
 with sigma of 0.04
 C16-C41 \\sim C16-C41A
 with sigma of 0.02
 C67-C82 \\sim C67A-C82A
 with sigma of 0.04
 C81-C87 \\sim C81A-C87A
 with sigma of 0.04
 C17-C74 \\sim C17-C74A
 with sigma of 0.04
 C81-C94 \\sim C81A-C94A
 with sigma of 0.04
 C87-C94 \\sim C87A-C94A
 with sigma of 0.04
 C36-C80 \\sim C36A-C80A
 with sigma of 0.02
 C13-C70 \\sim C13-C70A
 with sigma of 0.04
 C3-C25 \\sim C3-C25A
 with sigma of 0.02
 C70-C80 \\sim C70A-C80A
 with sigma of 0.04
 C25-C72 \\sim C25A-C72A
 with sigma of 0.02
 C25-C77 \\sim C25A-C77A
 with sigma of 0.02
 C41-C71 \\sim C41A-C71A
 with sigma of 0.02
 C25-C90 \\sim C25A-C90A
 with sigma of 0.02
 C16-C82 \\sim C16-C82A
 with sigma of 0.04
 C17-C48 \\sim C17-C48A
 with sigma of 0.02
 C17-C65 \\sim C17-C65A
 with sigma of 0.04
 C3-C72 \\sim C3-C72A
 with sigma of 0.04
 C65-C74 \\sim C65A-C74A
 with sigma of 0.04
 C3-C77 \\sim C3-C77A
 with sigma of 0.04
 C3-C90 \\sim C3-C90A
 with sigma of 0.04
 C72-C77 \\sim C72A-C77A
 with sigma of 0.04
 C72-C90 \\sim C72A-C90A
 with sigma of 0.04
 C77-C90 \\sim C77A-C90A
 with sigma of 0.04
 C36-C70 \\sim C36A-C70A
 with sigma of 0.02
 C36-C83 \\sim C36A-C83A
 with sigma of 0.02
 C33-C76 \\sim C33-C76A
 with sigma of 0.02
 C13-C80 \\sim C13-C80A
 with sigma of 0.04
 C33-C84 \\sim C33-C84A
 with sigma of 0.02
 C33-C89 \\sim C33-C89A
 with sigma of 0.02
 C70-C83 \\sim C70A-C83A
 with sigma of 0.04
 C80-C83 \\sim C80A-C83A
 with sigma of 0.04
 C41-C67 \\sim C41A-C67A
 with sigma of 0.02
 C41-C82 \\sim C41A-C82A
 with sigma of 0.02
 C16-C71 \\sim C16-C71A
 with sigma of 0.04
 C67-C71 \\sim C67A-C71A
 with sigma of 0.04
 C4-C28 \\sim C4-C28A
 with sigma of 0.02
 C71-C82 \\sim C71A-C82A
 with sigma of 0.04
 C28-C56 \\sim C28A-C56A
 with sigma of 0.02
 C48-C65 \\sim C48A-C65A
 with sigma of 0.02
 C28-C73 \\sim C28A-C73A
 with sigma of 0.02
 C48-C74 \\sim C48A-C74A
 with sigma of 0.02
 C28-C86 \\sim C28A-C86A
 with sigma of 0.02
 C17-C69 \\sim C17-C69A
 with sigma of 0.04
 C4-C56 \\sim C4-C56A
 with sigma of 0.04
 C65-C69 \\sim C65A-C69A
 with sigma of 0.04
 C4-C73 \\sim C4-C73A
 with sigma of 0.04
 C69-C74 \\sim C69A-C74A
 with sigma of 0.04
 C4-C86 \\sim C4-C86A
 with sigma of 0.04
 C56-C73 \\sim C56A-C73A
 with sigma of 0.04
 C56-C86 \\sim C56A-C86A
 with sigma of 0.04
 C73-C86 \\sim C73A-C86A
 with sigma of 0.04
 C18-C63 \\sim C18-C63A
 with sigma of 0.02
 C18-C68 \\sim C18-C68A
 with sigma of 0.02
 C18-C79 \\sim C18-C79A
 with sigma of 0.02
 C1A-C1E \\sim C1A-C1C \\sim C1F-C1D \\sim C1B-C1F \\sim C1C-C1E \\sim C1B-C1D
 with sigma of 0.04
 C19-C1F \\sim C19-C1B
 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1A
 with sigma of 0.02
 N31A-C34A \\sim N31-C34 \\sim N1-C43 \\sim N1A-C43A \\sim N37-C45 \\sim
N57-C38 \\sim N57A-C38A ~
 N37A-C45A
 with sigma of 0.04
3. Restrained planarity
 C19, C1A, C1B, C1C, C1D, C1E, C1F
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C22A \\sim C34A \\sim C43A \\sim N1A \\sim N31A \\sim N1 \\sim C22 \\sim N31
\\sim C34 \\sim C43: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
C19 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Cr1) = Uanis(Zn1)
Uanis(Cr2) = Uanis(Zn2)
Uanis(Cr3) = Uanis(Zn3)
Uanis(Cr4) = Uanis(Zn4)
Uanis(Cr5) = Uanis(Zn5)
Uanis(Cr6) = Uanis(Zn6)
Uanis(Cr7) = Uanis(Zn7)
Uanis(Cr8) = Uanis(Zn8)
5. 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
 C32, N37, C38, C45, N57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32A, N37A, C38A, C45A, N57A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22A, N1A, N31A, C34A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, N1, N31, C34, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C81, C87, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, C68, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76, C84, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C67, C71, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C72, C77, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C56, C73, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C70, C80, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C65, C69, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42A, C81A, C87A, C94A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C72A, C77A, C90A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76A, C84A, C89A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28A, C56A, C73A, C86A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63A, C68A, C79A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36A, C70A, C80A, C83A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41A, C67A, C71A, C82A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48A, C65A, C69A, C74A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Cr3)+Sof(Zn3)]+1*[Sof(Cr7)+Sof(Zn7)]+1*[Sof(Cr8)+Sof(Zn8)]+1*[Sof(Cr6)+
 Sof(Zn6)]+1*[Sof(Cr2)+Sof(Zn2)]+1*[Sof(Cr5)+Sof(Zn5)]+1*[Sof(Cr1)+Sof(Zn1)]+1*
 [Sof(Cr4)+Sof(Zn4)]=6 with esd of 0
 Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C87A)=Sof(H87D)=Sof(H87E)=
 Sof(H87F)=Sof(C81A)=Sof(H81D)=Sof(H81E)=Sof(H81F)=Sof(C42A)=1-FVAR(1)
 Sof(C42)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C87)=Sof(H87A)=Sof(H87B)=
 Sof(H87C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=FVAR(1)
 Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=Sof(C72A)=Sof(H72D)=Sof(H72E)=
 Sof(H72F)=Sof(C25A)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=1-FVAR(2)
 Sof(C25)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(H77C)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(2)
 Sof(C84A)=Sof(H84D)=Sof(H84E)=Sof(H84F)=Sof(C89A)=Sof(H89D)=Sof(H89E)=
 Sof(H89F)=Sof(C76A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=1-FVAR(3)
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=FVAR(3)
 Sof(C86A)=Sof(H86D)=Sof(H86E)=Sof(H86F)=Sof(C73A)=Sof(H73D)=Sof(H73E)=
 Sof(H73F)=Sof(C28A)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(4)
 Sof(C28)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C73)=Sof(H73A)=Sof(H73B)=
 Sof(H73C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=FVAR(4)
 Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C68A)=Sof(H68D)=Sof(H68E)=
 Sof(H68F)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(5)
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(5)
 Sof(C36A)=Sof(C83A)=Sof(H83D)=Sof(H83E)=Sof(H83F)=Sof(C80A)=Sof(H80D)=
 Sof(H80E)=Sof(H80F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(6)
 Sof(C36)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(6)
 Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C67A)=Sof(H67D)=Sof(H67E)=
 Sof(H67F)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C41A)=1-FVAR(7)
 Sof(C41)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C71)=Sof(H71A)=Sof(H71B)=
 Sof(H71C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(7)
 Sof(C48A)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=Sof(C65A)=Sof(H65D)=
 Sof(H65E)=Sof(H65F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=1-FVAR(8)
 Sof(C48)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(8)
 Sof(C45A)=Sof(H45A)=Sof(C32A)=Sof(H32A)=Sof(N37A)=Sof(H37A)=Sof(N57A)=
 Sof(H57A)=Sof(C38A)=Sof(H38A)=1-FVAR(9)
 Sof(C32)=Sof(H32)=Sof(N37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C45)=Sof(H45)=
 Sof(N57)=Sof(H57)=FVAR(9)
 Sof(Zn3)=1-FVAR(10)
 Sof(Cr3)=FVAR(10)
 Sof(Zn7)=1-FVAR(11)
 Sof(Cr7)=FVAR(11)
 Sof(Zn8)=1-FVAR(12)
 Sof(Cr8)=FVAR(12)
 Sof(Zn6)=1-FVAR(13)
 Sof(Cr6)=FVAR(13)
 Sof(Zn2)=1-FVAR(14)
 Sof(Cr2)=FVAR(14)
 Sof(Zn5)=1-FVAR(15)
 Sof(Cr5)=FVAR(15)
 Sof(Zn1)=1-FVAR(16)
 Sof(Cr1)=FVAR(16)
 Sof(Zn4)=1-FVAR(17)
 Sof(Cr4)=FVAR(17)
 Sof(C34A)=Sof(H34A)=Sof(C43A)=Sof(H43A)=Sof(N31A)=Sof(H31A)=Sof(C22A)=
 Sof(H22A)=Sof(N1A)=Sof(H1A)=1-FVAR(18)
 Sof(C22)=Sof(H22)=Sof(N1)=Sof(H1)=Sof(N31)=Sof(H31)=Sof(C34)=Sof(H34)=
 Sof(C43)=Sof(H43)=FVAR(18)
 Fixed Sof: C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C1A(0.5) C1B(0.5) H1B(0.5)
 C1C(0.5) H1C(0.5) C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5)
7.a Free rotating group:
 C19(C1A,C1B,C1C,C1D,C1E,C1F)
7.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C94(H94A,H94B,
 H94C), C94A(H94D,H94E,H94F), C87A(H87D,H87E,H87F), C81A(H81D,H81E,H81F),
 C90A(H90D,H90E,H90F), C72A(H72D,H72E,H72F), C77A(H77D,H77E,H77F), C84A(H84D,
 H84E,H84F), C89A(H89D,H89E,H89F), C76A(H76D,H76E,H76F), C86A(H86D,H86E,H86F),
 C73A(H73D,H73E,H73F), C56A(H56D,H56E,H56F), C79A(H79D,H79E,H79F), C68A(H68D,
 H68E,H68F), C63A(H63D,H63E,H63F), C83A(H83D,H83E,H83F), C80A(H80D,H80E,H80F),
 C70A(H70D,H70E,H70F), C82A(H82D,H82E,H82F), C67A(H67D,H67E,H67F), C71A(H71D,
 H71E,H71F), C74A(H74D,H74E,H74F), C65A(H65D,H65E,H65F), C69A(H69D,H69E,H69F)
7.c Aromatic/amide H refined with riding coordinates:
 C22(H22), N1(H1), N31(H31), C32(H32), C34(H34), N37(H37), C38(H38), C43(H43),
 C45(H45), N57(H57), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F),
 C45A(H45A), C32A(H32A), N37A(H37A), N57A(H57A), C38A(H38A), C34A(H34A),
 C43A(H43A), N31A(H31A), C22A(H22A), N1A(H1A)
7.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              14633
_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 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.772