Rotaxanes composed of dibenzo-24-crown-8 and macrocyclic transition metal complexing tetraimine units
Tomczyk, Karolina; Wozny, Mateusz; Domagala, Slawomir; Wieckowska, Agnieszka; Pawłowska, Joanna; Wozniak, Krzysztof; Korybut-Daszkiewicz, Bohdan; New J. Chem. 41 (2017) 6004–6013; doi:10.1039/C7NJ00909G

data_7056229
_publ_section_title
;
 Rotaxanes composed of dibenzo-24-crown-8 and macrocyclic transition metal
 complexing tetraimine units
;
_journal_issue                   13
_journal_name_full               'New J. Chem.'
_journal_page_first              6004
_journal_page_last               6013
_journal_paper_doi               10.1039/C7NJ00909G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety
'C40 H58 N12 Ni2, 4(F6 P), C24 H32 O8, 0.5 (C2 H3 N), C H2 Cl2'
_chemical_formula_sum            'C66 H93.5 Cl2 F24 N12.5 Ni2 O8 P4'
_chemical_formula_weight         1958.23
_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
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-01-29 deposited with the CCDC.
2017-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                76.752(3)
_cell_angle_beta                 87.027(3)
_cell_angle_gamma                81.031(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7226(4)
_cell_length_b                   16.6566(6)
_cell_length_c                   20.9375(6)
_cell_measurement_reflns_used    24515
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5020
_cell_measurement_theta_min      2.1220
_cell_volume                     4265.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4391
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313  125.0000  -30.0000 94

  2 omega  -50.00   34.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313   38.0000  120.0000 84

  3 omega  -50.00   34.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313   38.0000  -30.0000 84

  4 omega -121.00    0.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313  -19.0000  150.0000 121

  5 omega   23.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5313 -125.0000 -150.0000 74

  6 omega   23.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5313 -125.0000 -120.0000 74

  7 omega   84.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -60.0000 94

  8 omega   39.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 59

  9 omega   36.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  150.0000 109

 10 omega   84.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -180.0000 94

 11 omega   86.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 92

 12 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 80

 13 omega   39.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -150.0000 59

 14 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 55

 15 omega   84.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 94

 16 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 80

 17 omega   36.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 80

 18 omega  100.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -150.0000 78

 19 omega   36.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 74

 20 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 80

 21 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -120.0000 80

 22 omega   39.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 59

 23 omega   36.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 80

 24 omega   80.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.0000   17.8353 98

 25 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   34.0000 -116.3766 91

 26 omega   36.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -120.0000 74

 27 omega   36.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -30.0000 80

 28 omega   36.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 80

 29 omega   39.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 59

 30 omega   59.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000    0.0000 119

 31 omega   36.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -30.0000 109

 32 omega  -69.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313   57.0000 -150.0000 102

 33 omega -113.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313  -57.0000   60.0000 101

 34 omega -117.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313  -77.0000    0.0000 109

 35 omega -113.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.5313  -57.0000  150.0000 101

 36 omega    8.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5313   77.0000    0.0000 109

 37 omega    8.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5313   77.0000  -90.0000 109

 38 omega    4.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5313   88.0000  142.5464 29

 39 omega   81.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   71.0000  -15.4426 97

 40 omega   82.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   64.0000 -165.5586 96

 41 omega   83.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -120.0000 60

 42 omega   83.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   59.0000   73.6045 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1174481000
_diffrn_orient_matrix_UB_12      0.0014251000
_diffrn_orient_matrix_UB_13      -0.0154380000
_diffrn_orient_matrix_UB_21      -0.0254963000
_diffrn_orient_matrix_UB_22      0.0910424000
_diffrn_orient_matrix_UB_23      0.0071715000
_diffrn_orient_matrix_UB_31      0.0242453000
_diffrn_orient_matrix_UB_32      0.0306652000
_diffrn_orient_matrix_UB_33      -0.0736600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            89025
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.168
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             2014
_exptl_crystal_size_max          0.5022
_exptl_crystal_size_mid          0.2952
_exptl_crystal_size_min          0.2037
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.715
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.635
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         15599
_refine_ls_number_restraints     724
_refine_ls_restrained_S_all      1.684
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.1061
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3443
_refine_ls_wR_factor_ref         0.3602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12831
_reflns_number_total             15599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00909g2.cif
_cod_data_source_block           rx-para-nini
_cod_database_code               7056229
_chemical_oxdiff_formula         'C50 H100 N4 P4 F24 Ni2'
_cell_oxdiff_angle_alpha         76.752(3)
_cell_oxdiff_angle_beta          87.027(3)
_cell_oxdiff_angle_gamma         81.031(3)
_cell_oxdiff_length_a            12.7226(4)
_cell_oxdiff_length_b            16.6566(6)
_cell_oxdiff_length_c            20.9375(6)
_cell_oxdiff_measurement_reflns_used 24515
_cell_oxdiff_volume              4265.5(2)
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-H31B
 2 with sigma of 0.04
 Cl1-C65 \\sim Cl2-C65
 with sigma of 0.02
 F3B-F4B \\sim F4B-F5B \\sim F5B-F6B \\sim F6B-F3B
 with sigma of 0.02
 F19B-F20B \\sim F19B-F22B
 with sigma of 0.02
 C54-C55 \\sim C56-C55 \\sim C56-C57 \\sim C54-C53 \\sim C57-C58 \\sim C44-C45
\\sim C43-C44 \\sim C43-C42
 \\sim C42-C41 \\sim C45-C46
 with sigma of 0.02
 P4A-F22A \\sim P4A-F24A \\sim P4A-F21A \\sim P4A-F20A \\sim P4A-F23A \\sim
P4A-F19A
 with sigma of 0.02
 P4A-F22A \\sim P4A-F23A
 with sigma of 0.02
 P4B-F22B \\sim P4B-F20B \\sim P4B-F24B \\sim P4B-F21B \\sim P4B-F23B \\sim
P4B-F19B
 with sigma of 0.02
 C31A-C6 \\sim C31B-C4
 with sigma of 0.02
 Ni2B-N6B \\sim Ni2B-N7B \\sim Ni2B-N8B \\sim Ni2B-N9B \\sim Ni2A-N9A \\sim
Ni2A-N6A \\sim Ni2A-N7A ~
 Ni2A-N8A
 with sigma of 0.02
 N8B-C21B \\sim N8A-C21A \\sim N7A-C19A \\sim N7B-C19B \\sim N6A-C16A \\sim
N6B-C16B \\sim N9B-C24B ~
 N9A-C24A
 with sigma of 0.02
 C23B-C22B \\sim C23A-C22A \\sim C18B-C17B \\sim C18A-C17A
 with sigma of 0.02
 C21B-C20B \\sim C20B-C19B \\sim C20A-C19A \\sim C21A-C20A \\sim C25A-C16A
\\sim C25B-C16B \\sim C25A-
 C24A \\sim C25B-C24B
 with sigma of 0.02
 N7A-C18A \\sim N7B-C18B \\sim N6A-C17A \\sim N6B-C17B \\sim N9B-C23B \\sim
N8B-C22B \\sim N8A-C22A ~
 N9A-C23A
 with sigma of 0.02
 C26B-C25B \\sim C26A-C25A \\sim C40-C20A
 with sigma of 0.02
 N10A-C26A \\sim N10B-C26B \\sim N12-C40
 with sigma of 0.02
 N8B-C21B \\sim N7B-C19B \\sim N6B-C16B \\sim N9B-C24B
 with sigma of 0.02
 C21B-C19B \\sim C16B-C24B
 with sigma of 0.02
 C40-C20B \\sim C40-C20A
 with sigma of 0.02
 P1-F3B \\sim P1-F6B \\sim P1-F6A \\sim P1-F3A \\sim P1-F5B \\sim P1-F5A \\sim
P1-F4B \\sim P1-F4A
 with sigma of 0.02
 C23B-N8B \\sim C22B-N9B \\sim N6B-C18B \\sim N7B-C17B
 with sigma of 0.02
 N8B-N7B \\sim N9B-N6B
 with sigma of 0.02
 N8B-N9B \\sim N6B-N7B
 with sigma of 0.02
 N11B-C31B \\sim N11A-C31A
 with sigma of 0.02
3. Restrained planarity
 Ni2B, N6B, N7B, N8B, N9B
 with sigma of 0.1
 N10B, C16B, C25B, C26B, C27B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N10B \\sim C26B \\sim C27B \\sim C28B \\sim C29B \\sim C30B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C66) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C67) \\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P4A, P1, P3, P4B, P2, F19A, F20A, F21A, F22A, F23A, F24A, F1, F2, F3A, F3B,
 F4A, F4B, F5A, F5B, F6A, F6B, F13, F14, F15, F16, F17, F18, F19B, F20B, F21B,
 F22B, F23B, F24B, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl2, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, C66, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N11B)=Sof(H11B)=Sof(H32c)=Sof(H32d)=Sof(C31B)=Sof(H31B)=1-FVAR(1)
 Sof(N11A)=Sof(H11A)=Sof(C31A)=Sof(H31A)=Sof(H32a)=Sof(H32b)=FVAR(1)
 Sof(Ni2B)=Sof(N6B)=Sof(N7B)=Sof(N8B)=Sof(N9B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=
 Sof(H17c)=Sof(H17d)=Sof(C18B)=Sof(H18c)=Sof(H18d)=Sof(C19B)=Sof(H19B)=
 Sof(C20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22c)=Sof(H22d)=Sof(C23B)=
 Sof(H23c)=Sof(H23d)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(C26B)=Sof(H26B)=
 Sof(N10B)=Sof(C27B)=Sof(H27a)=Sof(H27b)=Sof(C28B)=Sof(H28a)=Sof(H28b)=
 Sof(H28c)=Sof(C29B)=Sof(H29a)=Sof(H29b)=Sof(C30B)=Sof(H30a)=Sof(H30b)=
 Sof(H30c)=Sof(H40a)=1-FVAR(2)
 Sof(Ni2A)=Sof(N6A)=Sof(N7A)=Sof(N8A)=Sof(N9A)=Sof(N10A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17a)=Sof(H17b)=Sof(C18A)=Sof(H18a)=Sof(H18b)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22a)=Sof(H22b)=
 Sof(C23A)=Sof(H23a)=Sof(H23b)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27c)=Sof(H27d)=Sof(C28A)=Sof(H28d)=Sof(H28e)=
 Sof(H28f)=Sof(C29A)=Sof(H29c)=Sof(H29d)=Sof(C30A)=Sof(H30d)=Sof(H30e)=
 Sof(H30f)=Sof(H40)=FVAR(2)
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(3)
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(3)
 Sof(P4B)=Sof(F19B)=Sof(F20B)=Sof(F21B)=Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(4)
 Sof(P4A)=Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=FVAR(4)
 Fixed Sof: N13(0.5) C66(0.5) H66a(0.5) H66b(0.5) H66c(0.5) C67(0.5)
7.a Free rotating group:
 N13(C31B)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C7(H7a,H7b), C8(H8a,H8b), C12(H12a,H12b), C14(H14a,
 H14b), C17A(H17a,H17b), C17B(H17c,H17d), C18A(H18a,H18b), C18B(H18c,H18d),
 C22A(H22a,H22b), C22B(H22c,H22d), C23A(H23a,H23b), C23B(H23c,H23d), C27B(H27a,
 H27b), C29B(H29a,H29b), C27A(H27c,H27d), C29A(H29c,H29d), C32(H32a,H32b),
 C32(H32c,H32d), C39(H39a,H39b), C47(H47a,H47b), C48(H48a,H48b), C49(H49a,H49b),
  C50(H50a,H50b), C51(H51a,H51b), C52(H52a,H52b), C59(H59a,H59b), C60(H60a,
 H60b), C61(H61a,H61b), C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b),
 C65(H65a,H65b)
7.c Me refined with riding coordinates:
 C28B(H28a,H28b,H28c), C30B(H30a,H30b,H30c)
7.d Aromatic/amide H refined with riding coordinates:
 N11A(H11A), N11B(H11B), N12(H12), C1(H1), C4(H4), C6(H6), C9(H9), C11(H11),
 C16A(H16A), C16B(H16B), C19A(H19A), C19B(H19B), C21A(H21A), C21B(H21B),
 C24A(H24A), C24B(H24B), C26A(H26A), C26B(H26B), C31A(H31A), C34(H34), C35(H35),
  C37(H37), C38(H38), C40(H40a), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C54(H54), C55(H55), C56(H56), C57(H57), C31B(H31B)
7.e Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C28A(H28d,H28e,H28f), C30A(H30d,
 H30e,H30f), C66(H66a,H66b,H66c)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'