Conformational flexibility of hybrid [3]- and [4]-rotaxanes.
Lockyer, Selena J.; Nawaz, Selina; Brookfield, Adam; Fielding, Alistair J.; Vitorica-Yrezabal, Inigo J; Timco, Grigore A.; Burton, Neil A.; Bowen, Alice M.; Winpenny, Richard E. P.; McInnes, Eric J. L.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c06547

data_4135222
_publ_section_title
;
 Conformational flexibility of hybrid [3]- and [4]-rotaxanes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c06547
_journal_year                    2020
_chemical_formula_moiety
'3(C80 H144 Cr8 F8 O32), C75 H111 Cr3 N6 O13 S3'
_chemical_formula_sum            'C315 H543 Cr27 F24 N6 O109 S3'
_chemical_formula_weight         8114.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.1390(6)
_cell_length_b                   52.7563(9)
_cell_length_c                   30.1676(8)
_cell_measurement_reflns_used    31649
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      20.4190
_cell_measurement_theta_min      3.3820
_cell_volume                     47967.2(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.581
_diffrn_measured_fraction_theta_max 0.995
_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    -94.00 -61.00   0.75   45.82    --  -17.77-178.00  90.00   44
  2  \w    -47.00  74.50   0.75   45.82    --   18.86   0.00 120.00  162
  3  \w     29.00  90.50   0.75   45.82    --   18.86  19.00 -30.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0194685000
_diffrn_orient_matrix_UB_12      0.0055764000
_diffrn_orient_matrix_UB_13      0.0089297000
_diffrn_orient_matrix_UB_21      -0.0065788000
_diffrn_orient_matrix_UB_22      0.0038108000
_diffrn_orient_matrix_UB_23      -0.0215710000
_diffrn_orient_matrix_UB_31      -0.0114966000
_diffrn_orient_matrix_UB_32      -0.0116211000
_diffrn_orient_matrix_UB_33      -0.0027566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.1292
_diffrn_reflns_Laue_measured_fraction_full 0.581
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62221
_diffrn_reflns_point_group_measured_fraction_full 0.571
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             17036
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 4864 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2436
_refine_ls_number_reflns         24813
_refine_ls_number_restraints     8496
_refine_ls_restrained_S_all      2.859
_refine_ls_R_factor_all          0.1879
_refine_ls_R_factor_gt           0.1471
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3688
_refine_ls_wR_factor_ref         0.4074
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.560
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                16183
_reflns_number_total             24813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c06547_si_003.cif
_cod_data_source_block           arepw1244
_cod_database_code               4135222
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cr8Ni3F9O32N2C100H200
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.718
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1_1-C2_1
 C1_2-C2_2
 C1_3-C2_3
 C1_4-C2_4
 C1_5-C2_5
 C1_6-C2_6
 C1_7-C2_7
 C1_8-C2_8
 C1_9-C2_9
 C1_10-C2_10
 C1_11-C2_11
 C1_12-C2_12
 C1_13-C2_13
 C1_14-C2_14
 C1_15-C2_15
 C1_16-C2_16
 C1_17-C2_17
 C1_18-C2_18
 C1_19-C2_19
 C1_20-C2_20
 C1_21-C2_21
 C1_22-C2_22
 C1_23-C2_23
 C1_25-C2_25
 C1_26-C2_26
 C1_27-C2_27
 1.5 with sigma of 0.02
 C1CA-C0CA
 2.4 with sigma of 0.02
 S35-C32 = S27-C24
 1.7 with sigma of 0.01
 C17-C18 = C17-C14
 1.5 with sigma of 0.02
 C5A-C4A
 2.4 with sigma of 0.01
 C50-C56
 2.4 with sigma of 0.02
 C50-C52
 2.4 with sigma of 0.02
 S27-C28 = S57-C58
 1.8 with sigma of 0.02
 C4BA-C1_24
 2.4 with sigma of 0.002
 C4_24-C3_24 = C5_24-C3_24 = C4BA-C3_24
 1.5 with sigma of 0.02
 N19-C18
 1.45 with sigma of 0.02
 C2_19-C1_19
 1.5 with sigma of 0.02
 C2_3-C1_3
 1.5 with sigma of 0.02
 C4A-C3A
 2.4 with sigma of 0.02
 C4A-C5A
 2.4 with sigma of 0.02
 C5A-C3A
 2.4 with sigma of 0.02
 O2_25-C1_25 \\sim O2A-C1_25 \\sim O1A-C1_25 \\sim O1_25-C1_25
 with sigma of 0.01
 C3BA-C1BA \\sim C1BA-C9AA
 with sigma of 0.02
 C1BA-C9AA \\sim C9AA-C3BA
 with sigma of 0.02
 C3BA-C1_25 \\sim C1_25-C9AA
 with sigma of 0.02
 C3BA-C1_25 \\sim C1_25-C1BA
 with sigma of 0.02
 S35-C32 \\sim S27-C24
 with sigma of 0.01
 S35-C36 \\sim S27-C28
 with sigma of 0.01
 S57-C58 \\sim S27_$1-C28_$1
 with sigma of 0.01
 C55-S57 \\sim S57-C53
 with sigma of 0.02
 C58-C54 \\sim C32-C36 \\sim C28-C24
 with sigma of 0.002
 C2_3-C1_3 \\sim C2A-C1_3 \\sim C4A-C2A \\sim C4_3-C2_3 \\sim C3A-C2A \\sim
C5_3-C2_3 \\sim C5A-C2A ~
 C3_3-C2_3 \\sim C4_20-C2_20 \\sim C5_20-C2_20 \\sim C3_20-C2_20 \\sim
C2_20-C1_20 \\sim C8BA-C0CA
 \\sim C3_7-C2_7 \\sim C8BA-C1CA \\sim C9BA-C8BA \\sim C4_7-C2_7 \\sim
C3_25-C2_25 \\sim C9AA-C8AA ~
 C8AA-C1BA \\sim C5_25-C2_25 \\sim C8AA-C3BA \\sim C4_25-C2_25 \\sim
C2_25-C1_25 \\sim C8AA-C1_25 ~
 C4BA-C1_24
 with sigma of 0.01
 C17-C18 \\sim C48-C47
 with sigma of 0.01
 N49-C48 \\sim N49-C50_$1 \\sim N19-C18 \\sim N19-C20
 with sigma of 0.01
 N49-C50 \\sim N49-C48 \\sim N19-C20 \\sim N19-C18
 with sigma of 0.01
3. Restrained planarity
 S57, C54, C53, C52, C51, C56, C55
 with sigma of 0.1
 C50, C51, C56, C55, C54, C53, C52, S57
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2_25 \\sim C8AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C3BA \\sim C5_25 \\sim C1BA \\sim C3_25 \\sim C9AA: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C24 \\sim C32 \\sim C33 \\sim C25 \\sim C26 \\sim C34 \\sim C21 \\sim C29 \\sim
C30 \\sim C22 \\sim C23 \\sim C31: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
S27 \\sim S35: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C36 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C4_8 \\sim C3_8 \\sim C5_8: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C53 \\sim C52 \\sim C51 \\sim C56 \\sim C55 \\sim C54: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C58 \\sim S57 \\sim C54: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
C1_9 \\sim O1_9 \\sim O2_9 \\sim C2_9 \\sim C4_9 \\sim C5_9 \\sim C3_9: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C42 \\sim N41 \\sim C46 \\sim C45 \\sim C44 \\sim C43: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C5_21, Cr07, F00L, F00P, O2_4, O2_21, O2_26, O2_27, Cr0B, Cr0D, C1_4, C1_21,
 C1_26, C1_27, O1_21, O1_27, F00N, O1_4, O1_18, O1_22, O1_26, C2_4, C2_21,
 C2_26, C2_27, Cr0C, C1_18, C1_22, C3_4, C4_4, C5_4, C3_21, C4_21, C3_26, C4_26,
  C5_26, C3_27, C4_27, C5_27, F00M, O2_9, O2_18, O2_22, O2_23, C2_18, C2_22,
 C1_9, C1_23, C3_18, C4_18, C5_18, C3_22, C4_22, C5_22, O1_9, C2_9, O1_23,
 C2_23, C3_9, C4_9, C5_9, C3_23, C4_23, C5_23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C28, S27, S35, C36, C24, C31, C30, C22, C21, C29, C34, C26, C25, C33, C32,
 C20, N19, C18, C17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4_1, C5_1, C3_1, C2_1, C1_1, O1_1, O2_1, Cr9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4_8, C3_8, C5_8, C2_8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F1, Cr6, F6, F5, O2_2, O1_5, O2_13, O2_17, Cr7, Cr5, C1_2, C1_5, C1_13, C1_17,
  F7, O1_2, O2_5, O1_6, O1_19, F4, O1A, O1_13, O1_17, O1_24, O1_25, C2_2, C2_5,
 C2_13, C2_17, Cr8, C1_6, C1_19, Cr4, C1_25, C1_24, C3_2, C4_2, C5_2, C3_5,
 C4_5, C5_5, C3_13, C4_13, C5_13, C3_17, C4_17, C5_17, F8, O2_3, O2_6, O2_12,
 O2_19, C2_6, C4AA, C2_19, F3, O2A, O1_7, O2_14, O2_24, O2_25, C8AA, C2_25,
 C4BA, Cr1, C1_3, C1_12, C3_6, C4_6, C5_6, C5AA, C6AA, C7AA, C3_19, C4_19,
 C5_19, Cr3, C1_7, C1_14, C9AA, C1BA, C3BA, C3_25, C4_25, C5_25, C3_24, C4_24,
 C5_24, O1_3, O2_11, O1_12, O2_20, C2A, C2_3, C2_12, F2, O2_7, O1_14, O2_15,
 O2_16, C8BA, C2_7, C2_14, Cr2, C1_11, C1_20, C5A, C4A, C3A, C3_3, C4_3, C5_3,
 C3_12, C4_12, C5_12, C1_15, C1_16, C9BA, C0CA, C1CA, C3_7, C4_7, C5_7, C3_14,
 C4_14, C5_14, O1_11, O1_15, O1_16, O1_20, C2_11, C2_20, C2_15, C2_16, C3_11,
 C4_11, C5_11, C3_20, C4_20, C5_20, C3_15, C4_15, C5_15, C3_16, C4_16, C5_16
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cr9, Cr10, O100, N11, N41, O1_1, O2_1, C1_1, C2_1, C3_1, C5_2, O1_8, O2_8,
 C1_8, C2_8, C3_8, C5_8, O1_10, O2_10, C1_10, C2_10, C3_10, C4_10, C5_10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N41, C42, C43, C44, C45, C51, C52, C55, C54, C53, C56, S57, C50, C47, C48,
 N49, C58
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{O1_2, O2_2, C1_2, C2_2, C3_2, C4_2, C5_2}
{O1_3, O2_3, C1_3, C2_3, C3_3, C4_3, C5_3}
{O1_4, O2_4, C1_4, C2_4, C3_4, C4_4, C5_4}
{O1_5, O2_5, C1_5, C2_5, C3_5, C4_5, C5_5}
{O1_6, O2_6, C1_6, C2_6, C3_6, C4_6, C5_6}
{O1_7, O2_7, C1_7, C2_7, C3_7, C4_7, C5_7}
{O1_8, O2_8, C1_8, C2_8, C3_8, C4_8, C5_8}
{O1_9, O2_9, C1_9, C2_9, C3_9, C4_9, C5_9}
{O1_10, O2_10, C1_10, C2_10, C3_10, C4_10, C5_10}
{O1_11, O2_11, C1_11, C2_11, C3_11, C4_11, C5_11}
{O1_12, O2_12, C1_12, C2_12, C3_12, C4_12, C5_12}
{O1_13, O2_13, C1_13, C2_13, C3_13, C4_13, C5_13}
{O1_14, O2_14, C1_14, C2_14, C3_14, C4_14, C5_14}
{O1_15, O2_15, C1_15, C2_15, C3_15, C4_15, C5_15}
{O1_16, O2_16, C1_16, C2_16, C3_16, C4_16, C5_16}
{O1_17, O2_17, C1_17, C2_17, C3_17, C4_17, C5_17}
{O1_18, O2_18, C1_18, C2_18, C3_18, C4_18, C5_18}
{O1_19, O2_19, C1_19, C2_19, C3_19, C4_19, C5_19}
{O1_20, O2_20, C1_20, C2_20, C3_20, C4_20, C5_20}
{O1_21, O2_21, C1_21, C2_21, C3_21, C4_21, C5_21}
{O1_22, O2_22, C1_22, C2_22, C3_22, C4_22, C5_22}
{O1_23, O2_23, C1_23, C2_23, C3_23, C4_23, C5_23}
{O1_25, O2_25, C1_25, C2_25, C3_25, C4_25, C5_25}
{O1_26, O2_26, C1_26, C2_26, C3_26, C4_26, C5_26}
{O1_27, O2_27, C1_27, C2_27, C3_27, C4_27, C5_27}
as
{O1_1, O2_1, C1_1, C2_1, C3_1, C4_1, C5_1} sigma for 1-2: 0.02 1-3: 0.04
7. Others
 Sof(C2A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(C4AA)=Sof(C5AA)=Sof(H5AD)=Sof(H5AE)=Sof(H5AF)=Sof(C6AA)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(2)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
 Sof(C8AA)=Sof(O1A)=Sof(O2A)=Sof(C9AA)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C1BA)=
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C3BA)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=1-FVAR(3)
 Sof(O1)=Sof(O2)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(3)
 Sof(C8BA)=Sof(C9BA)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C0CA)=Sof(H0CA)=
 Sof(H0CB)=Sof(H0CC)=Sof(C1CA)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(4)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(4)
 Sof(H20C)=Sof(H20D)=Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=
 Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(S35)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=1-FVAR(5)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(C25)=Sof(H25)=
 Sof(C26)=Sof(H26)=Sof(S27)=Sof(H20A)=Sof(H20B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(5)
 Fixed Sof: C53(0.5) H53(0.5) C52(0.5) H52(0.5) C51(0.5) C56(0.5) H56(0.5)
 C55(0.5) H55(0.5) C54(0.5) S57(0.5) C50(0.5) H50A(0.5) H50B(0.5) C47(0.5)
 H47A(0.5) H47B(0.5) C46(0.5) H46(0.5) N41(0.5) C42(0.5) H42(0.5) C43(0.5)
 H43(0.5) C44(0.5) C45(0.5) H45(0.5) H48A(0.5) H48B(0.5) N49(0.5) H49A(0.5)
 H49B(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) H1(0)
8.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C20(H20C,H20D), N19(H19A,H19B), C50(H50A,
 H50B), C17(H17A,H17B), C47(H47A,H47B), C48(H48A,H48B), N49(H49A,H49B)
8.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C58(H58A,H58B,H58C), C5A(H5AA,H5AB,H5AC), C4A(H4AA,H4AB,
 H4AC), C3A(H3AA,H3AB,H3AC), C5AA(H5AD,H5AE,H5AF), C6AA(H6AA,H6AB,H6AC),
 C7AA(H7AA,H7AB,H7AC), C9AA(H9AA,H9AB,H9AC), C1BA(H1BA,H1BB,H1BC), C3BA(H3BA,
 H3BB,H3BC), C4BA(H4BA,H4BB,H4BC), C9BA(H9BA,H9BB,H9BC), C0CA(H0CA,H0CB,H0CC),
 C1CA(H1CA,H1CB,H1CC), C36(H36A,H36B,H36C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C4(H4A,H4B,
 H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,
 H4C), C5(H5A,H5B,H5C)
8.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C53(H53), C52(H52), C56(H56),
 C55(H55), C12(H12), C16(H16), C15(H15), C13(H13), C46(H46), C42(H42), C43(H43),
  C45(H45), C30(H30), C31(H31), C33(H33), C34(H34), C1(H1)
8.d Fitted hexagon refined as free rotating group:
 C21(C22,C23,C24,C25,C26), C53(C52,C51,C56,C55,C54), C12(N11,C16,C15,C14,C13),
 C46(N41,C42,C43,C44,C45), C29(C30,C31,C32,C33,C34)
;
_shelx_res_checksum              86759
_shelx_hkl_checksum              18579
_olex2_date_sample_data_collection 2016-08-10
_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 3.296
_oxdiff_exptl_absorpt_empirical_full_min 0.268