Templating metallocycles with a macrocycle: synthesis, structures and magnetic studies of {Cr<sub>11</sub>M<sub>2</sub>} complexes.
Alotaibi, Rajeh; Brookfield, Adam; Fowler, Jonathan M.; Whitehead, George F. S.; Lockyer, Selena J.; Timco, Grigore A.; Collison, David; Schnack, Jürgen; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 52 (2022) 20–23; doi:10.1039/d2dt03368b

data_7711856
_publ_section_title
;
 Templating metallocycles with a macrocycle: synthesis, structures and
 magnetic studies of {Cr<sub>11</sub>M<sub>2</sub>} complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20
_journal_page_last               23
_journal_paper_doi               10.1039/d2dt03368b
_journal_volume                  52
_journal_year                    2022
_chemical_formula_moiety         'C120 H222 Cr11 Cu2 F15 N4 O44, 0.5(C2 H3 N)'
_chemical_formula_sum            'C121 H223.5 Cr11 Cu2 F15 N4.5 O44'
_chemical_formula_weight         3429.61
_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     direct
_audit_creation_date             2022-10-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-05 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                71.668(2)
_cell_angle_beta                 73.433(2)
_cell_angle_gamma                70.962(2)
_cell_formula_units_Z            4
_cell_length_a                   21.8291(5)
_cell_length_b                   29.6847(7)
_cell_length_c                   31.7603(6)
_cell_measurement_reflns_used    24670
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.9960
_cell_measurement_theta_min      2.8190
_cell_volume                     18081.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -42.00   1.00   1.00   17.50    --  -18.04 -77.00 -90.00   43
  2  \w     -2.00  88.00   1.00   17.50    --   19.45  57.00-120.00   90
  3  \w     -6.00  38.00   1.00   17.50    --   19.45  77.00  90.00   44
  4  \w     15.00  88.00   1.00   17.50    --   19.45  57.00 120.00   73
  5  \w    -49.00  41.00   1.00   17.50    --   19.45 -57.00 -30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0091069000
_diffrn_orient_matrix_UB_12      0.0062997000
_diffrn_orient_matrix_UB_13      -0.0239860000
_diffrn_orient_matrix_UB_21      -0.0162315000
_diffrn_orient_matrix_UB_22      0.0250198000
_diffrn_orient_matrix_UB_23      -0.0002917000
_diffrn_orient_matrix_UB_31      0.0297681000
_diffrn_orient_matrix_UB_32      0.0037236000
_diffrn_orient_matrix_UB_33      0.0014137000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            78802
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        21.491
_diffrn_reflns_theta_max         21.491
_diffrn_reflns_theta_min         2.586
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             7160
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3942
_refine_ls_number_reflns         41387
_refine_ls_number_restraints     20734
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0874P)^2^+40.0270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27023
_reflns_number_total             41387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03368b2.cif
_cod_data_source_block           arepw1962
_cod_depositor_comments
'Adding full bibliography for 7711856--7711857.cif.'
_cod_original_cell_volume        18081.3(8)
_cod_original_formula_sum        'C121 H223.50 Cr11 Cu2 F15 N4.50 O44'
_cod_database_code               7711856
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Restrained distances
 Cu2-N4A \\sim Cu2-N1 \\sim Cu2-N4 \\sim Cu2-N3A \\sim Cu2-N2A \\sim Cu2-N2
\\sim Cu2-N3 \\sim Cu2-N1A
 with sigma of 0.02
 C72-C71 \\sim C72A-C71
 with sigma of 0.02
 C97-C244 \\sim C97A-C244
 with sigma of 0.02
 C37A-C36 \\sim C37-C36
 with sigma of 0.02
 C77A-C76 \\sim C77-C76
 with sigma of 0.02
 C67-C66 \\sim C67A-C66
 with sigma of 0.02
 C52A-C51 \\sim C52-C51
 with sigma of 0.02
 C87A-C86 \\sim C87-C86
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Cu2 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim C221 \\sim C222 \\sim C223 \\sim
C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228 \\sim C229 \\sim C230 \\sim
N1A \\sim N2A \\sim N3A \\sim N4A \\sim C241 \\sim C1A \\sim C1B \\sim C1C
\\sim C1D \\sim C1F \\sim C1G \\sim C1H \\sim C1I \\sim C1E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C244 \\sim
C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C221
\\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228
\\sim C229 \\sim C230 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115
\\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122
\\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129
\\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136
\\sim C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143
\\sim C144 \\sim C145 \\sim C146 \\sim C147 \\sim C148 \\sim C149 \\sim C150
\\sim C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156 \\sim C157
\\sim C158 \\sim C159 \\sim C160 \\sim C161 \\sim C162 \\sim C163 \\sim C164
\\sim C165 \\sim C166 \\sim C167 \\sim C168 \\sim C169 \\sim C170 \\sim C171
\\sim C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176 \\sim C177 \\sim C178
\\sim C179 \\sim C180 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C185
\\sim C186 \\sim C187 \\sim C188 \\sim C189 \\sim C190 \\sim C191 \\sim C192
\\sim C193 \\sim C194 \\sim C195 \\sim C196 \\sim C197 \\sim C198 \\sim C199
\\sim C200 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206
\\sim C207 \\sim C208 \\sim C209 \\sim C210 \\sim C211 \\sim C212 \\sim C213
\\sim C214 \\sim C215 \\sim C216 \\sim C217 \\sim C218 \\sim C219 \\sim C220
\\sim C231 \\sim C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C237
\\sim C238 \\sim C239 \\sim C240 \\sim C241 \\sim C1A \\sim C1B \\sim C1C \\sim
C1D \\sim C1E \\sim C1F \\sim C1G \\sim C1H \\sim C1I \\sim C243 \\sim C242
\\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C67A \\sim C68A \\sim C69A
\\sim C70A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim C87A \\sim C88A
\\sim C89A \\sim C90A \\sim C77A \\sim C78A \\sim C79A \\sim C80A \\sim C97A
\\sim C98A \\sim C99A \\sim C96 \\sim C72A \\sim C73A \\sim C74A \\sim C75A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cu2, N1, N3, N4, C221, C226, C227, C228, C229, C230, N2A, N3A, N4A, C1C, C1D,
 C1E, C1F, C1G, N2, C223, C224, C225, N1A, C241, C1A, C1I, C222, C1B, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79,
 C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95,
  C244, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108,
 C109, C110, C221, C222, C223, C224, C225, C226, C227, C228, C229, C230, C111,
 C112, C113, C114, C115, C116, C117, C118, C119, C120, C121, C122, C123, C124,
 C125, C126, C127, C128, C129, C130, C131, C132, C133, C134, C135, C136, C137,
 C138, C139, C140, C141, C142, C143, C144, C145, C146, C147, C148, C149, C150,
 C151, C152, C153, C154, C155, C156, C157, C158, C159, C160, C161, C162, C163,
 C164, C165, C166, C167, C168, C169, C170, C171, C172, C173, C174, C175, C176,
 C177, C178, C179, C180, C181, C182, C183, C184, C185, C186, C187, C188, C189,
 C190, C191, C192, C193, C194, C195, C196, C197, C198, C199, C200, C201, C202,
 C203, C204, C205, C206, C207, C208, C209, C210, C211, C212, C213, C214, C215,
 C216, C217, C218, C219, C220, C231, C232, C233, C234, C235, C236, C237, C238,
 C239, C240, C241, C1A, C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I, C243, C242,
 C37A, C38A, C39A, C40A, C67A, C68A, C69A, C70A, C52A, C53A, C54A, C55A, C87A,
 C88A, C89A, C90A, C77A, C78A, C79A, C80A, C97A, C98A, C99A, C96, C72A, C73A,
 C74A, C75A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
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
{O17, O18, C41, C42, C43, C44, C45}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19, O20, C46, C47, C48, C49, C50}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21, O22, C51, C52, C53, C54, C55}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23, O24, C56, C57, C58, C59, C60}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25, O26, C61, C62, C63, C64, C65}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27, O28, C66, C67, C68, C69, C70}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29, O30, C71, C72, C73, C74, C75}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31, O32, C76, C77, C78, C79, C80}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O33, O34, C81, C82, C83, C84, C85}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O35, O36, C86, C87, C88, C89, C90}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O37, O38, C91, C92, C93, C94, C95}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O39, O40, C244, C97, C98, C99, C100}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O41, O42, C101, C102, C103, C104, C105}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O43, O44, C106, C107, C108, C109, C110}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O45, O46, C111, C112, C113, C114, C115}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O47, O48, C116, C117, C118, C119, C120}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O49, O50, C121, C122, C123, C124, C125}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O51, O52, C126, C127, C128, C129, C130}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O53, O54, C131, C132, C133, C134, C135}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O55, O56, C136, C137, C138, C139, C140}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O57, O58, C141, C142, C143, C144, C145}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O59, O60, C146, C147, C148, C149, C150}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O61, O62, C151, C152, C153, C154, C155}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O63, O64, C156, C157, C158, C159, C160}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O65, O66, C161, C162, C163, C164, C165}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O67, O68, C166, C167, C168, C169, C170}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O69, O70, C171, C172, C173, C174, C175}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O71, O72, C176, C177, C178, C179, C180}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O73, O74, C181, C182, C183, C184, C185}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O75, O76, C186, C187, C188, C189, C190}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O77, O78, C191, C192, C193, C194, C195}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O79, O80, C196, C197, C198, C199, C200}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O81, O82, C201, C202, C203, C204, C205}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O83, O84, C206, C207, C208, C209, C210}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O85, O86, C211, C212, C213, C214, C215}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O87, O88, C216, C217, C218, C219, C220}
{Cu2, N1, N2, N3, N4, C221, C222, C223, C224, C225, C226, C227, C228, C229,
C230} sigma for 1-2: 0.02, 1-3: 0.04
as in
{Cu4, N5, N6, N7, N8, C231, C232, C233, C234, C235, C236, C237, C238, C239,
C240}
{N1, N2, N3, N4, C221, C222, C223, C224, C225, C226, C227, C228, C229, C230}
sigma for 1-2: 0.02, 1-3: 0.04
as in
{N1A, N2A, N3A, N4A, C241, C1A, C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C37A, C38A, C39A, C40A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C67A, C68A, C69A, C70A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C52A, C53A, C54A, C55A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C87A, C88A, C89A, C90A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C77A, C78A, C79A, C80A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C97A, C98A, C99A, C96}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C72A, C73A, C74A, C75A}
5. Others
 Sof(N1A)=Sof(H1A)=Sof(N2A)=Sof(H2A)=Sof(N3A)=Sof(H3AA)=Sof(N4A)=Sof(H4AA)=
 Sof(C241)=Sof(H24D)=Sof(H24E)=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(C1E)=
 Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=Sof(H1GA)=Sof(H1GB)=
 Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=1-FVAR(1)
 Sof(N1)=Sof(H1)=Sof(N2)=Sof(H2)=Sof(N3)=Sof(H3)=Sof(N4)=Sof(H4)=Sof(C221)=
 Sof(H22A)=Sof(H22B)=Sof(C222)=Sof(H22C)=Sof(H22D)=Sof(C223)=Sof(H22E)=
 Sof(H22F)=Sof(C224)=Sof(H22G)=Sof(H22H)=Sof(C225)=Sof(H22I)=Sof(H22J)=
 Sof(C226)=Sof(H22K)=Sof(H22L)=Sof(C227)=Sof(H22M)=Sof(H22N)=Sof(C228)=
 Sof(H22O)=Sof(H22P)=Sof(C229)=Sof(H22Q)=Sof(H22R)=Sof(C230)=Sof(H23D)=
 Sof(H23E)=FVAR(1)
 Sof(C37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(C67A)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69D)=
 Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(3)
 Sof(C67)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(3)
 Sof(C52A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(4)
 Sof(C52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(4)
 Sof(C87A)=Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C89A)=Sof(H89D)=
 Sof(H89E)=Sof(H89F)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(5)
 Sof(C87)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(H89A)=Sof(H89B)=
 Sof(H89C)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(5)
 Sof(C77A)=Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(C79A)=Sof(H79D)=
 Sof(H79E)=Sof(H79F)=Sof(C80A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(6)
 Sof(C77)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=
 Sof(H79C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(6)
 Sof(C97A)=Sof(C98A)=Sof(H98D)=Sof(H98E)=Sof(H98F)=Sof(C99A)=Sof(H99D)=
 Sof(H99E)=Sof(H99F)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=1-FVAR(7)
 Sof(C97)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C99)=Sof(H99A)=Sof(H99B)=
 Sof(H99C)=Sof(C100)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(7)
 Sof(C72A)=Sof(C73A)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C74A)=Sof(H74D)=
 Sof(H74E)=Sof(H74F)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(8)
 Sof(C72)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=Sof(H74A)=Sof(H74B)=
 Sof(H74C)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(8)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N1A(H1A),
 N2A(H2A), N3A(H3AA), N4A(H4AA)
6.b Secondary CH2 refined with riding coordinates:
 C221(H22A,H22B), C222(H22C,H22D), C223(H22E,H22F), C224(H22G,H22H), C225(H22I,
 H22J), C226(H22K,H22L), C227(H22M,H22N), C228(H22O,H22P), C229(H22Q,H22R),
 C230(H23D,H23E), C231(H23F,H23G), C232(H23H,H23I), C233(H23J,H23K), C234(H23L,
 H23M), C235(H23N,H23O), C236(H23P,H23Q), C237(H23R,H23S), C238(H23T,H23U),
 C239(H23V,H23W), C240(H24F,H24G), C241(H24D,H24E), C1A(H1AA,H1AB), C1B(H1BA,
 H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1F(H1FA,H1FB),
 C1G(H1GA,H1GB), C1H(H1HA,H1HB), C1I(H1IA,H1IB)
6.c Me refined with riding coordinates:
 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), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C83(H83A,
 H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C100(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C105(H10M,
 H10N,H10O), C108(H10P,H10Q,H10R), C109(H10S,H10T,H10U), C110(H11A,H11B,H11C),
 C113(H11D,H11E,H11F), C114(H11G,H11H,H11I), C115(H11J,H11K,H11L), C118(H11M,
 H11N,H11O), C119(H11P,H11Q,H11R), C120(H12A,H12B,H12C), C123(H12D,H12E,H12F),
 C124(H12G,H12H,H12I), C125(H12J,H12K,H12L), C128(H12M,H12N,H12O), C129(H12P,
 H12Q,H12R), C130(H13D,H13E,H13F), C133(H13G,H13H,H13I), C134(H13J,H13K,H13L),
 C135(H13M,H13N,H13O), C138(H13P,H13Q,H13R), C139(H13S,H13T,H13U), C140(H14D,
 H14E,H14F), C143(H14G,H14H,H14I), C144(H14J,H14K,H14L), C145(H14M,H14N,H14O),
 C148(H14P,H14Q,H14R), C149(H14S,H14T,H14U), C150(H15D,H15E,H15F), C153(H15G,
 H15H,H15I), C154(H15J,H15K,H15L), C155(H15M,H15N,H15O), C158(H15P,H15Q,H15R),
 C159(H15S,H15T,H15U), C160(H16A,H16B,H16C), C163(H16D,H16E,H16F), C164(H16G,
 H16H,H16I), C165(H16J,H16K,H16L), C168(H16M,H16N,H16O), C169(H16P,H16Q,H16R),
 C170(H17A,H17B,H17C), C173(H17D,H17E,H17F), C174(H17G,H17H,H17I), C175(H17J,
 H17K,H17L), C178(H17M,H17N,H17O), C179(H17P,H17Q,H17R), C180(H18D,H18E,H18F),
 C183(H18G,H18H,H18I), C184(H18J,H18K,H18L), C185(H18M,H18N,H18O), C188(H18P,
 H18Q,H18R), C189(H18S,H18T,H18U), C190(H19D,H19E,H19F), C193(H19G,H19H,H19I),
 C194(H19J,H19K,H19L), C195(H19M,H19N,H19O), C198(H19P,H19Q,H19R), C199(H19S,
 H19T,H19U), C200(H20D,H20E,H20F), C203(H20G,H20H,H20I), C204(H20J,H20K,H20L),
 C205(H20M,H20N,H20O), C208(H20P,H20Q,H20R), C209(H20S,H20T,H20U), C210(H21A,
 H21B,H21C), C213(H21D,H21E,H21F), C214(H21G,H21H,H21I), C215(H21J,H21K,H21L),
 C218(H21M,H21N,H21O), C219(H21P,H21Q,H21R), C220(H22S,H22T,H22U), C38A(H38D,
 H38E,H38F), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F), C68A(H68D,H68E,H68F),
 C69A(H69D,H69E,H69F), C70A(H70D,H70E,H70F), C53A(H53D,H53E,H53F), C54A(H54D,
 H54E,H54F), C55A(H55D,H55E,H55F), C88A(H88D,H88E,H88F), C89A(H89D,H89E,H89F),
 C90A(H90D,H90E,H90F), C78A(H78D,H78E,H78F), C79A(H79D,H79E,H79F), C80A(H80D,
 H80E,H80F), C98A(H98D,H98E,H98F), C99A(H99D,H99E,H99F), C96(H96A,H96B,H96C),
 C73A(H73D,H73E,H73F), C74A(H74D,H74E,H74F), C75A(H75D,H75E,H75F)
6.d Idealised Me refined with riding coordinates:
 C243(H24H,H24I,H24J)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 195 electrons were 
found in a volume of 2469\%A^3^ in 11 voids per unit cell. 
This is consistent with the presence of 
0.5[C2H3N], 0.5[C2H3N], 0.5[C2H3N], 0.75[C2H3N] per Asymmetric Unit 
which account for 198 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22821
_shelx_hkl_checksum              76788
_shelx_fab_checksum              36148
_olex2_date_sample_data_collection 2020-09-30
_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 1.189
_oxdiff_exptl_absorpt_empirical_full_min 0.845