Structural Characterisation and Dynamics of a Paramagnetic {Cr12Ni3} Seahorse in Non-Crystalline Phases
Geue, Niklas; Hicks, Emily; Lockyer, Selena; Nawaz, Selina; Churchill, Olivia; Whitehead, George F. S.; Timco, Grigore A.; Burton, Neil A.; Barran, Perdita; Winpenny, Richard E. P.; Physical Chemistry Chemical Physics  (2024) –; doi:10.1039/D4CP04498C

data_7250000
_publ_section_title
;
 Structural Characterisation and Dynamics of a Paramagnetic {Cr12Ni3}
 Seahorse in Non-Crystalline Phases
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D4CP04498C
_journal_year                    2024
_chemical_formula_moiety
'2(C68 H128 Cr6 F9 N4 Ni1.5 O24), H2 O, 4.446(C2 H3 N), 4.554(C7 H8)'
_chemical_formula_sum            'C176.77 H307.77 Cr12 F18 N12.44 Ni3 O49'
_chemical_formula_weight         4533.71
_chemical_name_common            Seahorse
_chemical_name_systematic        '[{Ni(cyclen)}2Cr12NiF18(O2CtBu)24]'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-11-12 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                109.178(2)
_cell_angle_beta                 95.520(2)
_cell_angle_gamma                103.904(2)
_cell_formula_units_Z            2
_cell_length_a                   19.7601(4)
_cell_length_b                   24.4796(5)
_cell_length_c                   26.5191(5)
_cell_measurement_reflns_used    44711
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      29.0080
_cell_measurement_theta_min      1.7320
_cell_volume                     11544.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.804
_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     -4.00  92.00   1.00    3.00    --    7.60   0.00 -60.00   96
  2  \w    -56.00  47.00   1.00    3.00    --    7.60  60.00-120.00  103
  3  \w     70.00  97.00   1.00    3.00    --    7.60  60.00-120.00   27
  4  \w    -80.00   4.00   1.00    3.00    --    7.60  60.00 150.00   84
  5  \w    -80.00   1.00   1.00    3.00    --    7.60  40.00  30.00   81
  6  \w     60.00  86.00   1.00    3.00    --    7.60  40.00  30.00   26
  7  \w    -73.00 -36.00   1.00    3.00    --    7.60   0.00 -60.00   37
;
_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      -0.0095634000
_diffrn_orient_matrix_UB_12      0.0115359000
_diffrn_orient_matrix_UB_13      0.0256743000
_diffrn_orient_matrix_UB_21      -0.0219197000
_diffrn_orient_matrix_UB_22      0.0140707000
_diffrn_orient_matrix_UB_23      -0.0109146000
_diffrn_orient_matrix_UB_31      -0.0291085000
_diffrn_orient_matrix_UB_32      -0.0263809000
_diffrn_orient_matrix_UB_33      -0.0073482000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            160385
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.571
_diffrn_reflns_theta_min         1.575
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
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    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             4763
_exptl_crystal_size_max          0.586
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.224
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2867
_refine_ls_number_reflns         56991
_refine_ls_number_restraints     11344
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1134P)^2^+13.4835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                39452
_reflns_number_total             56991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04498c2.cif
_cod_data_source_block           s6278l
_cod_original_cell_volume        11544.3(4)
_cod_database_code               7250000
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.633
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{C38, C38A}
3. Restrained distances
 C151-C06Z
 1.54 with sigma of 0.02
 C162-C161
 1.54 with sigma of 0.02
 C06K-C06B
 1.54 with sigma of 0.02
 C142-C06J
 1.54 with sigma of 0.02
 C06Y-C138
 1.54 with sigma of 0.02
 C148-C147
 1.54 with sigma of 0.02
 C158-C157
 1.54 with sigma of 0.02
 C35A-C34 \\sim C35-C34
 with sigma of 0.02
 C146-C162 \\sim C162-C144
 with sigma of 0.02
 C50-C165 \\sim C50A-C165
 with sigma of 0.02
 C78-C77 \\sim C78A-C77
 with sigma of 0.02
 C20A-C19 \\sim C20-C19
 with sigma of 0.02
 C30A-C29 \\sim C30-C29
 with sigma of 0.02
 C118-C117 \\sim C166-C117
 with sigma of 0.02
 C152-C151 \\sim C151-C06E
 with sigma of 0.02
 C06P-C06B \\sim C06B-C06Q
 with sigma of 0.02
 C160-C142 \\sim C142-C0
 with sigma of 0.02
 C06I-C138 \\sim C138-C06N
 with sigma of 0.02
 C49-C148 \\sim C148-C149
 with sigma of 0.02
 C159-C158 \\sim C158-C153
 with sigma of 0.02
 N8-C74 \\sim N8-C75 \\sim N5-C76 \\sim N5-C69 \\sim N7-C73 \\sim N7-C72 \\sim
N6-C71 \\sim N6-C70
 with sigma of 0.02
 C72-C71 \\sim C74-C73 \\sim C76-C75 \\sim C70-C69
 with sigma of 0.02
 N5-C69 \\sim N5A-C69A \\sim N5A-C76A \\sim N5-C76 \\sim N6-C70 \\sim N6A-C70A
\\sim N6-C71 \\sim N6A-C71A
 \\sim N7A-C72A \\sim N7-C72 \\sim N7-C73 \\sim N7A-C73A \\sim N8A-C74A \\sim
N8-C74 \\sim N8-C75 \\sim N8A-C75A
 with sigma of 0.02
 C76A-C75A \\sim C76-C75 \\sim C74A-C73A \\sim C74-C73 \\sim C72-C71 \\sim
C72A-C71A \\sim C70A-C69A ~
 C70-C69
 with sigma of 0.02
 Ni3-N7A \\sim Ni3-N7
 with sigma of 0.02
 Ni3-N5A \\sim Ni3-N5
 with sigma of 0.02
 Ni3-N6 \\sim Ni3-N6A
 with sigma of 0.02
 Ni3-N8A \\sim Ni3-N8
 with sigma of 0.02
4. Restrained planarity
 C161, C145, C211, C235, C146, C144, C162
 with sigma of 0.01
 C06Z, C072, C150, C152, C05X, C06E, C151
 with sigma of 0.01
 C06K, C06B, C06P, C06Q, C06T, C139, C137
 with sigma of 0.01
 C06J, C142, C160, C0, C06O, C05Z, C1A
 with sigma of 0.01
 C06N, C063, C05Y, C06Y, C066, C06I, C138
 with sigma of 0.01
 C147, C148, C149, C49, C143, C163, C164
 with sigma of 0.01
 C158, C157, C153, C154, C155, C156, C159
 with sigma of 0.01
5. 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
C35A \\sim C35 \\sim C38A \\sim C38 \\sim C36A \\sim C36 \\sim C37 \\sim C37A:
within 2.6A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2.6A
Uanis(C162) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C38) = Uanis(C38A)
6. 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
7. Same fragment restrains
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, O4, C14, C15, C16, C17, C18}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, O8, C24, C25, C26, C27, C28}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19, O20, C54, C55, C56, C57, C58}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, O6, C19, C20, C21, C22, C23}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13, O14, C39, C40, C41, C42, C43}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, O10, C29, C30, C31, C32, C33}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31, O32, C92, C93, C94, C95, C96}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, O12, C34, C35, C36, C37, C38}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O47, O48, C132, C133, C134, C135, C136}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15, O16, C44, C45, C46, C47, C48}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25, O26, C77, C78, C79, C80, C81}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17, O18, C165, C50, C51, C52, C53}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C30A, C31A, C32A, C33A}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21, O22, C59, C60, C61, C62, C63}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O43, O44, C122, C123, C124, C125, C126}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23, O24, C64, C65, C66, C67, C68}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O37, O38, C107, C108, C109, C110, C111}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27, O28, C82, C83, C84, C85, C86}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C50A, C51A, C52A, C53A}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C166, C1B, C1C, C1D}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O45, O46, C127, C128, C129, C130, C131}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O33, O34, C97, C98, C99, C100, C101}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C20A, C21A, C22A, C23A}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O35, O36, C102, C103, C104, C105, C106}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C35A, C36A, C37A, C38A}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O39, O40, C112, C113, C114, C115, C116}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O41, O42, C117, C118, C119, C120, C121}
{O1, O2, C9, C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29, O30, C87, C88, C89, C90, C91}
{C10, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C78A, C79A, C80A, C81A}
8. Others
 Sof(C142)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C157)=Sof(C159)=Sof(H159)=
 Sof(C156)=Sof(H156)=Sof(C155)=Sof(H155)=Sof(C154)=Sof(H154)=Sof(C153)=
 Sof(H153)=Sof(C158)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C06J)=Sof(C160)=
 Sof(H160)=Sof(C06O)=Sof(H06O)=Sof(C1A)=Sof(H1AA)=Sof(C05Z)=Sof(H05Z)=Sof(C0)=
 Sof(H0)=1-FVAR(1)
 Sof(C06Y)=Sof(C06N)=Sof(H06N)=Sof(C063)=Sof(H063)=Sof(C05Y)=Sof(H05Y)=
 Sof(C066)=Sof(H066)=Sof(C06I)=Sof(H06I)=Sof(C138)=Sof(H13S)=Sof(H13T)=
 Sof(H13U)=Sof(C162)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C161)=Sof(C146)=
 Sof(H146)=Sof(C211)=Sof(H211)=Sof(C145)=Sof(H145)=Sof(C235)=Sof(H235)=
 Sof(C144)=Sof(H144)=FVAR(1)
 Sof(C147)=Sof(C149)=Sof(H149)=Sof(C143)=Sof(H143)=Sof(C164)=Sof(H164)=
 Sof(C163)=Sof(H163)=Sof(C49)=Sof(H49)=Sof(C148)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 1-FVAR(2)
 Sof(C141)=Sof(H14G)=Sof(H14H)=Sof(H14I)=Sof(N10)=Sof(C140)=FVAR(2)
 Sof(C20A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(3)
 Sof(C20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(3)
 Sof(C30A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(4)
 Sof(C30)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(4)
 Sof(C35A)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(5)
 Sof(C35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(5)
 Sof(C50A)=Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(6)
 Sof(C50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(6)
 Sof(C166)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=
 Sof(H1CC)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(7)
 Sof(C118)=Sof(C119)=Sof(H11P)=Sof(H11Q)=Sof(H11R)=Sof(C120)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C121)=Sof(H12D)=Sof(H12E)=Sof(H12F)=FVAR(7)
 Sof(C78A)=Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C80A)=Sof(H80D)=
 Sof(H80E)=Sof(H80F)=Sof(C81A)=Sof(H81D)=Sof(H81E)=Sof(H81F)=1-FVAR(8)
 Sof(C78)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=FVAR(8)
 Sof(N5A)=Sof(H5A)=Sof(N6A)=Sof(H6A)=Sof(N7A)=Sof(H7A)=Sof(N8A)=Sof(H8A)=
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=
 Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=Sof(C73A)=Sof(H73C)=
 Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75C)=Sof(H75D)=
 Sof(C76A)=Sof(H76C)=Sof(H76D)=1-FVAR(9)
 Sof(N5)=Sof(H5)=Sof(N6)=Sof(H6)=Sof(N7)=Sof(H7)=Sof(N8)=Sof(H8)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=FVAR(9)
 Sof(Ni3A)=1-FVAR(10)
 Sof(Ni3)=FVAR(10)
9.a Free rotating group:
 O045(H04A,H04B)
9.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N5A(H5A),
 N6A(H6A), N7A(H7A), N8A(H8A)
9.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5B,H5C), C6(H6B,H6C),
 C7(H7B,H7C), C8(H8B,H8C), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C69A(H69C,H69D), C70A(H70C,H70D), C71A(H71C,H71D), C72A(H72C,H72D), C73A(H73C,
 H73D), C74A(H74C,H74D), C75A(H75C,H75D), C76A(H76C,H76D)
9.d Me refined with riding coordinates:
 C11(H11S,H11T,H11U), C12(H12S,H12T,H12U), C13(H13P,H13Q,H13R), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C), C86(H86A,H86B,H86C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C),
 C91(H91A,H91B,H91C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C104(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,H10N,H10O), C109(H10P,
 H10Q,H10R), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C114(H11G,H11H,H11I),
 C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C119(H11P,H11Q,H11R), C120(H12A,
 H12B,H12C), C121(H12D,H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,H12K,H12L),
 C126(H12M,H12N,H12O), C129(H12P,H12Q,H12R), C130(H13A,H13B,H13C), C131(H13D,
 H13E,H13F), C134(H13G,H13H,H13I), C135(H13J,H13K,H13L), C136(H13M,H13N,H13O),
 C06B(H06A,H06B,H06C), C138(H13S,H13T,H13U), C142(H14A,H14B,H14C), C151(H15A,
 H15B,H15C), C148(H14D,H14E,H14F), C158(H15D,H15E,H15F), C162(H16D,H16E,H16F),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C31A(H31D,
 H31E,H31F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C36A(H36D,H36E,H36F),
 C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F), C51A(H51D,H51E,H51F), C52A(H52D,
 H52E,H52F), C53A(H53D,H53E,H53F), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC),
 C1D(H1DA,H1DB,H1DC), C79A(H79D,H79E,H79F), C80A(H80D,H80E,H80F), C81A(H81D,
 H81E,H81F)
9.e Aromatic/amide H refined with riding coordinates:
 C06N(H06N), C063(H063), C05Y(H05Y), C066(H066), C06I(H06I), C152(H152),
 C072(H072), C150(H150), C05X(H05X), C06E(H06E), C06P(H06P), C06T(H06T),
 C137(H137), C139(H139), C06Q(H06Q), C149(H149), C143(H143), C164(H164),
 C163(H163), C49(H49), C159(H159), C156(H156), C155(H155), C154(H154),
 C153(H153), C160(H160), C06O(H06O), C1A(H1AA), C05Z(H05Z), C0(H0), C146(H146),
 C211(H211), C145(H145), C235(H235), C144(H144)
9.f Fitted hexagon refined as free rotating group:
 C06Y(C06N,C063,C05Y,C066,C06I), C06Z(C152,C072,C150,C05X,C06E), C06K(C06P,
 C06T,C137,C139,C06Q), C147(C149,C143,C164,C163,C49), C157(C159,C156,C155,C154,
 C153), C06J(C160,C06O,C1A,C05Z,C0), C161(C146,C211,C145,C235,C144)
9.g Idealised Me refined with riding coordinates:
 C059(H05A,H05B,H05C), C05L(H05D,H05E,H05F), C061(H06D,H06F,H06G), C06V(H06H,
 H06J,H06K), C141(H14G,H14H,H14I)
;
_shelx_res_checksum              54078
_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.725