Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A Structural and Spectroscopic Study
Muller, I.; Schneider, C.; Pietzonka, C.; Kraus, F.; Werncke, C.G.; Inorganics 7 (2019) 117–; doi:10.3390/inorganics7100117

data_1556442
_publ_section_title
;
 Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A
 Structural and Spectroscopic Study
;
_journal_name_full               Inorganics
_journal_page_first              117
_journal_paper_doi               10.3390/inorganics7100117
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C22 H44 N4 Si4 Zn, C16 H34 K O7'
_chemical_formula_sum            'C38 H78 K N4 O7 Si4 Zn'
_chemical_formula_weight         919.87
_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     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.423(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1899(7)
_cell_length_b                   18.4365(10)
_cell_length_c                   22.8273(13)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.26
_cell_volume                     5107.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            96672
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.134
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1330 before and 0.0638 after correction. The Ratio of minimum to maximum transmission is 0.8917. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     1954
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.1281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+100.8345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2596
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7347
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            K_18c6_Zn10.cif
_cod_data_source_block           k(18c6)zn10
_cod_database_code               1556442
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si6-C28
 1.8 with sigma of 0.02
 O14-C59 \\sim O14-C60 \\sim O12-C41 \\sim O12-C45 \\sim O10-C46 \\sim O10-C47
\\sim O8-C48 \\sim O8-C49 ~
 O6-C50 \\sim O6-C67 \\sim O3-C65 \\sim O3-C62
 with sigma of 0.02
 C59-C41 \\sim C45-C46 \\sim C47-C48 \\sim C49-C50 \\sim C67-C65 \\sim C62-C60
 with sigma of 0.02
 C41-C45 \\sim C46-C47 \\sim C48-C49 \\sim C50-C67 \\sim C65-C62 \\sim C60-C59
 with sigma of 0.04
 O14-C41 \\sim O12-C46 \\sim O10-C48 \\sim O8-C50 \\sim O6-C65 \\sim O3-C60
\\sim O12-C59 \\sim O10-C45 ~
 O8-C47 \\sim O6-C49 \\sim O3-C67 \\sim O14-C62
 with sigma of 0.04
 O4-C63 \\sim O4-C39 \\sim O5-C64 \\sim O5-C68 \\sim O7-C69 \\sim O7-C51 \\sim
O9-C52 \\sim O9-C53 \\sim O11-
 C55 \\sim O11-C56 \\sim O13-C57 \\sim O13-C40
 with sigma of 0.02
 C63-C64 \\sim C68-C69 \\sim C51-C52 \\sim C53-C55 \\sim C56-C57 \\sim C40-C39
 with sigma of 0.02
 C64-C68 \\sim C69-C51 \\sim C52-C53 \\sim C55-C56 \\sim C57-C40 \\sim C39-C63
 with sigma of 0.04
 O4-C64 \\sim O5-C69 \\sim O7-C52 \\sim O9-C55 \\sim O11-C57 \\sim O13-C39
\\sim O5-C63 \\sim O7-C68 \\sim O9-
 C51 \\sim O11-C53 \\sim O13-C56 \\sim O4-C40
 with sigma of 0.04
 Si1-C20 \\sim Si1-C19
 with sigma of 0.02
 C37-C38 \\sim C35-C36
 with sigma of 0.02
 O2-C38 \\sim O2-C35
 with sigma of 0.02
 C37-O2 \\sim O2-C36
 with sigma of 0.04
 C34-C33 \\sim C32-C31
 with sigma of 0.02
 O1-C33 \\sim O1-C32
 with sigma of 0.02
 C34-O1 \\sim O1-C31
 with sigma of 0.04
 Si3-N4 \\sim Si3A-N4
 with sigma of 0.02
 Si3-C23 \\sim Si3A-C23A
 with sigma of 0.02
 Si3-C24 \\sim Si3A-C24A
 with sigma of 0.02
 Si3-C25 \\sim Si3A-C25A
 with sigma of 0.02
 N4-C23 \\sim N4-C23A
 with sigma of 0.04
 N4-C24 \\sim N4-C24A
 with sigma of 0.04
 N4-C25 \\sim N4-C25A
 with sigma of 0.04
 C23-C24 \\sim C23A-C24A
 with sigma of 0.04
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C24-C25 \\sim C24A-C25A
 with sigma of 0.04
 N4-Si6 \\sim N4-Si6A
 with sigma of 0.02
 C28-Si6 \\sim C28A-Si6A
 with sigma of 0.02
 Si6-C27 \\sim Si6A-C27A
 with sigma of 0.02
 Si6-C30 \\sim Si6A-C30A
 with sigma of 0.02
 N4-C28 \\sim N4-C28A
 with sigma of 0.04
 N4-C27 \\sim N4-C27A
 with sigma of 0.04
 N4-C30 \\sim N4-C30A
 with sigma of 0.04
 C28-C27 \\sim C28A-C27A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C27-C30 \\sim C27A-C30A
 with sigma of 0.04
 Zn1-N1 \\sim Zn1-N1A
 with sigma of 0.02
 Zn1-N2 \\sim Zn1-N2A
 with sigma of 0.02
 N1-C1 \\sim N1A-C1A
 with sigma of 0.02
 N1-C5 \\sim N1A-C5A
 with sigma of 0.02
 N2-C6 \\sim N2A-C6A
 with sigma of 0.02
 N2-C10 \\sim N2A-C10A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 Zn1-C1 \\sim Zn1-C1A
 with sigma of 0.04
 Zn1-C5 \\sim Zn1-C5A
 with sigma of 0.04
 Zn1-C6 \\sim Zn1-C6A
 with sigma of 0.04
 Zn1-C10 \\sim Zn1-C10A
 with sigma of 0.04
 N1-C2 \\sim N1A-C2A
 with sigma of 0.04
 N1-C4 \\sim N1A-C4A
 with sigma of 0.04
 N1-C6 \\sim N1A-C6A
 with sigma of 0.04
 N2-C5 \\sim N2A-C5A
 with sigma of 0.04
 N2-C7 \\sim N2A-C7A
 with sigma of 0.04
 N2-C9 \\sim N2A-C9A
 with sigma of 0.04
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C1-C5 \\sim C1A-C5A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C6-C10 \\sim C6A-C10A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C8-C10 \\sim C8A-C10A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O3 \\sim O6 \\sim O8 \\sim O10 \\sim O12 \\sim O14 \\sim C41 \\sim C45 \\sim
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C59 \\sim C60 \\sim C62 \\sim
C65 \\sim C67: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O4 \\sim O5 \\sim O7 \\sim O9 \\sim O11 \\sim O13 \\sim C39 \\sim C40 \\sim C51
\\sim C52 \\sim C53 \\sim C55 \\sim C56 \\sim C57 \\sim C63 \\sim C64 \\sim C68
\\sim C69: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O2 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C23 \\sim C24 \\sim Si3 \\sim C25 \\sim N4 \\sim C30 \\sim Si6 \\sim C27:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C23 \\sim C24 \\sim Si3 \\sim C25: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N4 \\sim C27 \\sim Si6 \\sim C28 \\sim C30: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N1 \\sim N2 \\sim C1 \\sim H1 \\sim C2 \\sim H2 \\sim C3 \\sim H3 \\sim C4
\\sim H4 \\sim C5 \\sim C6 \\sim C7 \\sim H7 \\sim C8 \\sim H8 \\sim C9 \\sim
H9 \\sim C10 \\sim H10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N1A \\sim N2A \\sim C1A \\sim C2A \\sim H2A \\sim C3A \\sim H3A \\sim C4A \\sim
H4A \\sim C5A \\sim C6A \\sim C7A \\sim H7A \\sim C8A \\sim H8A \\sim C9A \\sim
H9A \\sim C10A \\sim H10A \\sim H1A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O14) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C59) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(C67) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C60)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O11) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(Si3) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(Si6) \\sim Ueq,
Uanis(C27) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(Si3) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N4) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(Si6) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(Si6) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.0002
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C10) \\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N1A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq,
Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A)
\\sim Ueq, Uanis(C10A) \\sim Ueq, : with sigma of 0.1 and sigma for terminal
atoms of 0.2
Uanis(C6) = Uanis(C2)
Uanis(C10) = Uanis(C1)
Uanis(C34) = Uanis(C31) = Uanis(C32) = Uanis(C33)
Uanis(O14) = Uanis(O4) = Uanis(O3) = Uanis(O5) = Uanis(O6) = Uanis(O7) =
Uanis(O8) = Uanis(O9) = Uanis(O10) = Uanis(O11) = Uanis(O12) = Uanis(O13)
Uanis(C40) = Uanis(C59) = Uanis(C41) = Uanis(C50) = Uanis(C39)
Uanis(C25) = Uanis(C24) = Uanis(C23)
Uanis(C35) = Uanis(C38)
Uanis(C24) = Uanis(C25A)
Uanis(C24A) = Uanis(C23)
Uanis(C23A) = Uanis(C25)
Uanis(Si3) = Uanis(Si1) = Uanis(Si3A)
Uanis(C1) = Uanis(C7)
Uanis(C22) = Uanis(C21)
Uanis(Si6A) = Uanis(Si6)
Uanis(C27A) = Uanis(C27)
Uanis(C30A) = Uanis(C30)
Uanis(N1A) = Uanis(N4)
Uanis(N1) = Uanis(N3)
Uanis(C3) = Uanis(C3A)
Uanis(C2A) = Uanis(C2)
4. Rigid body (RIGU) restrains
 O3, O6, O8, O10, O12, O14, C41, C45, C46, C47, C48, C49, C50, C59, C60, C62,
 C65, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, O7, O9, O11, O13, C39, C40, C51, C52, C53, C55, C56, C57, C63, C64,
 C68, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C24, Si3, C25, N4, C30, Si6, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C24, Si3, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C27, Si6, C28, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N2, C1, H1, C2, H2, C3, H3, C4, H4, C5, C6, C7, H7, C8, H8, C9, H9, C10,
 H10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1A, N2A, C1A, C2A, H2A, C3A, H3A, C4A, H4A, C5A, C6A, C7A, H7A, C8A, H8A,
 C9A, H9A, C10A, H10A, H1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Si3(0.5) N1(0.5) N2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5)
 H3(0.5) C4(0.5) H4(0.5) C5(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) Si6(0.5) C6(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) O1(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) O2(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) O3(0.5) O6(0.5) O8(0.5) O10(0.5) O12(0.5)
 O14(0.5) C41(0.5) H41A(0.5) H41B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5)
 H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C65(0.5)
 H65A(0.5) H65B(0.5) C67(0.5) H67A(0.5) H67B(0.5) O4(0.5) O5(0.5) O7(0.5)
 O9(0.5) O11(0.5) O13(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5)
 H64B(0.5) C68(0.5) H68A(0.5) H68B(0.5) C69(0.5) H69A(0.5) H69B(0.5) C23A(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
 Si3A(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C27A(0.5) H27D(0.5)
 H27E(0.5) H27F(0.5) Si6A(0.5) C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5)
 C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) N1A(0.5) N2A(0.5) C1A(0.5) H1A(0.5)
 C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) C6A(0.5)
 C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C38(H38A,H38B), C41(H41A,
 H41B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B),
  C65(H65A,H65B), C67(H67A,H67B), C39(H39A,H39B), C40(H40A,H40B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C63(H63A,H63B), C64(H64A,H64B), C68(H68A,H68B), C69(H69A,H69B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C1A(H1A),
 C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C),
 C30(H30A,H30B,H30C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C23A(H23D,H23E,H23F),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C27A(H27D,H27E,H27F), C28A(H28D,
 H28E,H28F), C30A(H30D,H30E,H30F)
;
_shelx_res_checksum              94340
_shelx_hkl_checksum              8677
_olex2_submission_special_instructions 'No special instructions were received'