Atomically accurate site-specific ligand tailoring of highly acid- and alkali-resistant Ti(iv)-based metallamacrocycle for enhanced CO<sub>2</sub> photoreduction.
Tian, Yi-Qi; Dai, Lin-Fang; Mu, Wen-Lei; Yu, Wei-Dong; Yan, Jun; Liu, Chao; Chemical science 14 (2023) 14280–14289; doi:10.1039/d3sc06046b

data_1570462
_publ_section_title
;
 Atomically accurate site-specific ligand tailoring of highly acid- and
 alkali-resistant Ti(iv)-based metallamacrocycle for enhanced
 CO<sub>2</sub> photoreduction.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              14280
_journal_page_last               14289
_journal_paper_doi               10.1039/d3sc06046b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C380 H452 Cl4 O72 Ti16, 30[H2O], 16[H2O], 2[H2O], 2[H2O]'
_chemical_formula_sum            'C380 H552 Cl4 O122 Ti16'
_chemical_formula_weight         7980.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-09 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.050(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.051(3)
_cell_length_b                   32.810(3)
_cell_length_c                   37.614(3)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      38.886
_cell_measurement_theta_min      3.068
_cell_volume                     43660(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ' 7.39 for PHOTON III'
_diffrn_detector_type            'Bruker Photon III 28'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON III 28detector'
_diffrn_measurement_method       'Profile data from \q/2\q scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1644
_diffrn_reflns_av_unetI/netI     0.1401
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            146370
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        42.494
_diffrn_reflns_theta_max         42.494
_diffrn_reflns_theta_min         2.359
_diffrn_source_current           3.57
_diffrn_source_power             0.24972149999999999
_diffrn_source_voltage           69.95
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  0.7483
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS, Madison WI for PHOTON III'
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             16912
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2481
_refine_ls_number_reflns         23005
_refine_ls_number_restraints     917
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.1329
_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^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3450
_refine_ls_wR_factor_ref         0.3742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13036
_reflns_number_total             23005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06046b2.cif
_cod_data_source_block           Ti16L4-1-HCla
_cod_depositor_comments
'Adding full bibliography for 1570454--1570469.cif.'
_cod_original_cell_volume        43661(6)
_cod_database_code               1570462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.563
_shelx_estimated_absorpt_t_min   0.411
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C81-C66
 1.45 with sigma of 0.01
 O2-C66
 1.5 with sigma of 0.01
 C95-C96
 2.3 with sigma of 0.01
 C66-C82
 1.45 with sigma of 0.01
 C86-C73
 1.5 with sigma of 0.01
 C91-C97
 2.3 with sigma of 0.01
 C25-C64
 2.3 with sigma of 0.01
 C25-C28
 2.3 with sigma of 0.01
 C42-C43
 1.5 with sigma of 0.01
 C78-C79
 1.5 with sigma of 0.01
 C80-C79
 1.5 with sigma of 0.01
 C87-C67
 2.3 with sigma of 0.01
 C74-C41
 2.3 with sigma of 0.01
 C27-C62 \\sim C27-C28
 with sigma of 0.02
 C27-C65 \\sim C27-C25
 with sigma of 0.02
 C27-C63 \\sim C27-C64
 with sigma of 0.02
 C31-C36 \\sim C31-C35
 with sigma of 0.02
 C31-C34 \\sim C31-C33
 with sigma of 0.02
 C31-C32 \\sim C31-C37
 with sigma of 0.02
 C48-C57 \\sim C48-C56
 with sigma of 0.02
 C48-C55 \\sim C48-C60
 with sigma of 0.02
 C48-C59 \\sim C48-C58
 with sigma of 0.02
 C51-C52 \\sim C51-C54
 with sigma of 0.02
 C51-C50 \\sim C51-C53
 with sigma of 0.02
 C51-C38 \\sim C51-C49
 with sigma of 0.02
 C04Z-C75 \\sim C04Z-C41
 with sigma of 0.02
 C04Z-C76 \\sim C04Z-C70
 with sigma of 0.02
 C04Z-C69 \\sim C04Z-C74
 with sigma of 0.02
 C86-C68 \\sim C86-C87
 with sigma of 0.02
 C86-C77 \\sim C86-C88
 with sigma of 0.02
 C86-C73 \\sim C86-C67
 with sigma of 0.02
 C20-C23 \\sim C20-C26
 with sigma of 0.02
 C20-C22 \\sim C20-C19
 with sigma of 0.02
 C20-C102 \\sim C20-C24
 with sigma of 0.02
 C13-C14 \\sim C12-C14
 with sigma of 0.02
 C104-C14 \\sim C103-C14
 with sigma of 0.02
 C11-C14 \\sim C105-C14
 with sigma of 0.02
 C21-C95 \\sim C21-C97
 with sigma of 0.02
 C21-C96 \\sim C21-C91
 with sigma of 0.02
 C21-C93 \\sim C21-C94
 with sigma of 0.02
 C98-C048 \\sim C99-C048
 with sigma of 0.02
 C100-C048 \\sim C84-C048
 with sigma of 0.02
 C048-C90 \\sim C048-C101
 with sigma of 0.02
 C72-C4 \\sim C72-C3
 with sigma of 0.02
 C72-C6 \\sim C72-C5
 with sigma of 0.02
 C72-C2 \\sim C72-C111
 with sigma of 0.02
3. Rigid bond restraints
 O2, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C111 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C98 \\sim C99 \\sim C100 \\sim C84 \\sim C90 \\sim C101: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C81 \\sim C66 \\sim C82 \\sim O2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C61 \\sim C27 \\sim C29 \\sim C30 \\sim C62 \\sim C63 \\sim C65 \\sim C64 \\sim
C25 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C21 \\sim C95 \\sim C96 \\sim C93: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C31 \\sim C32 \\sim C34 \\sim C36 \\sim C33 \\sim C35 \\sim C37: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C48 \\sim C55 \\sim C57 \\sim C59 \\sim C56 \\sim C58 \\sim C60: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C38 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C74 \\sim C75 \\sim C41 \\sim C76 \\sim C70 \\sim C69: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C77 \\sim C88 \\sim C73 \\sim C67 \\sim C68 \\sim C86 \\sim C87: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C78 \\sim C79 \\sim C80: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C19 \\sim C23 \\sim C26 \\sim C20 \\sim C22 \\sim C24 \\sim C102: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C103 \\sim C104 \\sim C105 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C91 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C98) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C106)
\\sim Ueq, Uanis(C107) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C111) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C62, C63, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C64, C25, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C34, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, C35, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C57, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C58, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C50, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C53, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C75, C76, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C70, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C77, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87, C88, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C22, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C19, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C104, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C103, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C95, C96, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C97, C91, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C98, C100, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C99, C84, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(1)
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=FVAR(1)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(2)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(2)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=1-FVAR(3)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(3)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(4)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(4)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=1-FVAR(5)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=FVAR(5)
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=1-FVAR(6)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(6)
 Sof(O2)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=Sof(C66)=Sof(H66)=1-FVAR(7)
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C79)=Sof(H79)=Sof(C78)=Sof(H78A)=
 Sof(H78B)=Sof(H78C)=Sof(O1)=FVAR(7)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(8)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C102)=Sof(H10L)=Sof(H10M)=Sof(H10N)=FVAR(8)
 Sof(C103)=Sof(H10O)=Sof(H10P)=Sof(H10Q)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C105)=Sof(H10R)=Sof(H10S)=Sof(H10T)=1-FVAR(9)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C104)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(9)
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=1-FVAR(10)
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(10)
 Sof(C101)=Sof(H10U)=Sof(H10V)=Sof(H10W)=Sof(C99)=Sof(H99A)=Sof(H99B)=
 Sof(H99C)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(11)
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C100)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(11)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C111)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(12)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(12)
 Fixed Sof: H1BC(0.75) H1BD(0.75) H1AA(0.25) H1AB(0.25) Cl3(0.75) Cl2(0.25)
7.a Riding coordinates:
 C04P(H04A,H04B,H04D), C71(H71A,H71B,H71C), C04Y(H04E,H04F,H04H), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C109(H10A,H10B,H10C), C05F(H05A,H05B,H05C),
 C05G(H05D,H05E,H05F), C4(H4A,H4B,H4C), C75(H75A,H75B,H75C), C18(H18A,H18B,
 H18C), C98(H98A,H98B,H98C), C05Q(H05G,H05H,H05I), C76(H76A,H76B,H76C),
 C83(H83A,H83B,H83C), C6(H6A,H6B,H6C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
  C100(H10D,H10E,H10F), C06C(H06A,H06B,H06C), C2(H2A,H2B,H2C), C52(H52A,H52B,
 H52C), C16(H16A,H16B,H16C), C50(H50A,H50B,H50C), C104(H10G,H10H,H10I),
 C69(H69A,H69B,H69C), C11(H11A,H11B,H11C), C044(H04M,H04N,H04O), C050(H05J,H05K,
 H05L), C68(H68A,H68B,H68C), C056(H05M,H05N,H05O), C059(H05P,H05Q,H05R),
 C90(H90A,H90B,H90C), C38(H38A,H38B,H38C), C102(H10L,H10M,H10N), C77(H77A,H77B,
 H77C), C85(H85A,H85B,H85C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,
 H59B,H59C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C),
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C56(H56A,H56B,
 H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C93(H93A,H93B,H93C), C25(H25A,H25B,H25C),
 C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C73(H73A,H73B,H73C), C49(H49A,H49B,H49C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C80(H80A,H80B,H80C), C78(H78A,H78B,H78C), C41(H41A,H41B,H41C),
 C70(H70A,H70B,H70C), C74(H74A,H74B,H74C), C88(H88A,H88B,H88C), C67(H67A,H67B,
 H67C), C87(H87A,H87B,H87C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C26(H26A,
 H26B,H26C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C103(H10O,H10P,H10Q),
 C12(H12A,H12B,H12C), C105(H10R,H10S,H10T), C97(H97A,H97B,H97C), C91(H91A,H91B,
 H91C), C94(H94A,H94B,H94C), C101(H10U,H10V,H10W), C99(H99A,H99B,H99C),
 C84(H84A,H84B,H84C), C5(H5A,H5B,H5C), C111(H11D,H11E,H11F), C3(H3A,H3B,H3C)
7.b Ternary CH refined with riding coordinates:
 C055(H055), C79(H79), C66(H66)
7.c Secondary CH2 refined with riding coordinates:
 C01I(H01A,H01B), C01S(H01C,H01D), C43(H43A,H43B), C02F(H02A,H02B), C02K(H02D,
 H02E), C03D(H03A,H03B), C03E(H03C,H03D), C03J(H03E,H03F), C03R(H03G,H03H),
 C03S(H03J,H03K), C03Y(H03L,H03M), C1(H1BC,H1BD), C1(H1AA,H1AB), C10(H10J,H10K),
  C028(H02F,H02G), C036(H03N,H03O), C039(H03P,H03Q), C040(H04I,H04K), C047(H04P,
 H04Q)
7.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C01T(H01T), C108(H108), C01Z(H01Z), C02C(H02C), C02M(H02M),
 C02N(H02N), C02O(H02O), C02U(H02U), C02W(H02W), C02X(H02X), C44(H44),
 C03I(H03I), C03X(H03X), C04C(H04C), C04G(H04G), C04J(H04J), C04L(H04L),
 C04S(H04S), C04W(H04W), C107(H107), C46(H46), C61(H61), C024(H024), C025(H025),
  C30(H30), C041(H041), C042(H042), C043(H043), C045(H045), C049(H049),
 C051(H051)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40848
_shelx_fab_checksum              860
_olex2_submission_special_instructions 'No special instructions were received'