Structural, thermal and topological characterization of coordination networks containing flexible aminocarboxylate ligands with a central biphenylene scaffold
Balestri, Davide; Scilabra, Patrick; Carraro, Claudia; Delledonne, Andrea; Bacchi, Alessia; Mazzeo, Paolo Pio; Carlucci, Lucia; Pelagatti, Paolo; CrystEngComm 21 (2019) 6365–; doi:10.1039/C9CE01230C

data_7233983
_publ_section_title
;
 Structural, thermal and topological characterization of coordination
 networks containing flexible aminocarboxylate ligands with a central
 biphenylene scaffold
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6365
_journal_paper_doi               10.1039/C9CE01230C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C104 H80 N8 O28 Zr6, 2(H2 O)'
_chemical_formula_sum            'C104 H84 N8 O30 Zr6'
_chemical_formula_weight         2473.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.16(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.551(1)
_cell_length_b                   24.348(2)
_cell_length_c                   19.579(1)
_cell_measurement_reflns_used    7200
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     9225.8(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  diffractometer
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.2309
_diffrn_reflns_av_unetI/netI     0.3197
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38188
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        21.618
_diffrn_reflns_theta_max         21.618
_diffrn_reflns_theta_min         1.035
_diffrn_source                   synchrotron
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  1
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.890
_exptl_crystal_description       'tiny needle'
_exptl_crystal_F_000             2488
_exptl_crystal_preparation       Solvothermal
_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.952
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         20493
_refine_ls_number_restraints     2450
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.3108
_refine_ls_R_factor_gt           0.1472
_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^)+(0.1400P)^2^+8.9990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3325
_refine_ls_wR_factor_ref         0.4094
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5628
_reflns_number_total             20493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01230c2.cif
_cod_data_source_block           Zr
_cod_depositor_comments
'Adding full bibliography for 7233980--7233983.cif.'
_cod_database_code               7233983
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(19)
 0.45(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O4-C52
 1.35 with sigma of 0.02
 O42-C52
 1.35 with sigma of 0.02
 C52-O4
 1.35 with sigma of 0.02
 C4-N1
 1.47 with sigma of 0.02
 N1-C7
 1.383 with sigma of 0.02
 C0AA-O3
 1.314 with sigma of 0.02
 C0AA-O1AA
 1.314 with sigma of 0.02
 O14-Zr1
 1.842 with sigma of 0.02
 Zr5-O14
 2.506 with sigma of 0.02
 O14-Zr4
 2.606 with sigma of 0.02
 C68-N6
 1.477 with sigma of 0.02
 N6-C71
 1.3 with sigma of 0.02
 C91-C88 = C13-C10 = C65-C62 = C39-C36
 1.5 with sigma of 0.02
 O5-C26
 1.35 with sigma of 0.02
 C26-O6
 1.342 with sigma of 0.02
 C26-O5
 1.364 with sigma of 0.02
 O5AA-C01
 1.361 with sigma of 0.02
 C01-O4AA
 1.351 with sigma of 0.02
 O4AA-C01
 1.351 with sigma of 0.02
 C01-O5AA
 1.361 with sigma of 0.02
 Zr3-O18
 1.913 with sigma of 0.02
 O18-Zr4
 2.091 with sigma of 0.02
 O18-Zr6
 2.549 with sigma of 0.02
 Zr3-O23
 2.145 with sigma of 0.02
 O23-Zr4
 2.404 with sigma of 0.02
 O23-Zr1
 2.4053 with sigma of 0.02
 Zr1-O23
 2.053 with sigma of 0.02
 O7-Zr5
 2.056 with sigma of 0.02
 O7-Zr6
 2.056 with sigma of 0.02
 O7-Zr4
 2.252 with sigma of 0.02
 Zr2-O102
 1.832 with sigma of 0.02
 O102-Zr6
 2.082 with sigma of 0.02
 O102-Zr5
 2.24 with sigma of 0.02
 C1AA-O46
 1.332 with sigma of 0.02
 C1AA-O88
 1.41 with sigma of 0.02
 C48-O3AA = C74-O0AA = C100-O19 = C22-O3
 2.4 with sigma of 0.04
 O16-C100 = C22-O1AA = C48-O8 = O49-C74
 2.4 with sigma of 0.04
 N1-C5
 -2.6 with sigma of 0.04
 N1-C3
 2.6 with sigma of 0.04
 C27-O6
 -2.4 with sigma of 0.04
 C27-O5
 -2.4 with sigma of 0.04
 C29-N3
 2.4 with sigma of 0.04
 C34-N3
 2.4 with sigma of 0.04
 C41-N4
 2.4 with sigma of 0.04
 C46-N4
 2.4 with sigma of 0.04
 N1-C12
 2.449 with sigma of 0.04
 N1-C8
 2.341 with sigma of 0.04
 C5-N1
 2.447 with sigma of 0.04
 C3-N1
 2.5907 with sigma of 0.04
 C15-N2
 2.279 with sigma of 0.04
 C17-N2
 2.402 with sigma of 0.04
 N2-C20
 2.408 with sigma of 0.04
 N2-C24
 2.524 with sigma of 0.04
 N6-C76
 2.352 with sigma of 0.04
 N6-C67
 2.583 with sigma of 0.04
 C6-C01 = C1AA-C80 = C0AA-C23 = C99-C2AA = C73-C77 = C52-C54 = C26-C32 = C49-C51
 2.4 with sigma of 0.04
 C47-C51 = C77-C75 = C58-C52 = C28-C26 = C2-C01 = C1AA-C84 = C101-C2AA = C21-
 C0AA
 2.4 with sigma of 0.04
 O4AA-O5AA
 2.484 with sigma of 0.04
 O46-C79
 2.416 with sigma of 0.04
 O88-C79
 2.576 with sigma of 0.04
 N2-C19 \\sim N2-C16 \\sim N1-C7 \\sim N1-C4 \\sim N7-C85 \\sim N7-C82 \\sim
N8-C94 \\sim N8-C97 \\sim N5-C56
 \\sim N5-C59 \\sim N3-C30 \\sim N3-C33 \\sim N4-C42 \\sim N4-C45 \\sim N6-C68
\\sim N6-C71
 with sigma of 0.02
 C51-C48 \\sim C77-C74 \\sim C27-C26 \\sim C53-C52 \\sim C2AA-C100 \\sim
C79-C1AA \\sim C1-C01 \\sim C22-
 C0AA
 with sigma of 0.02
 O14-Zr4 \\sim O18-Zr6
 with sigma of 0.02
 O5-C26 \\sim O6-C26 \\sim O4-C52 \\sim O42-C52 \\sim O46-C1AA \\sim O4AA-C01
\\sim O5AA-C01 \\sim O8-C51
 \\sim O3AA-C51 \\sim O49-C77 \\sim O0AA-C77 \\sim O19-C2AA \\sim O16-C2AA
\\sim O1AA-C0AA \\sim O3-C0AA
 with sigma of 0.02
4. Restrained atomic chiral volume
 C2AA
 fixed at 0 with sigma of 0.1
 C77
 fixed at 0 with sigma of 0.1
 C19, C16, C13, C10, C7, C4, C82, C85, C88, C91, C94, C97, C56, C59, C62, C65,
 C68, C71, C45, C42, C39, C36, C33, C30
 fixed at 0 with sigma of 0.1
 C79, C1AA, C1, C01, C27, C26, C52, C53, C22, C0AA, C74, C48, C51
 fixed at 0 with sigma of 0.1
 C27, C26
 fixed at 0 with sigma of 0.01
 C26
 fixed at 0 with sigma of 0.01
5. Restrained planarity
 N3, C33, C36, C39
 with sigma of 0.1
6. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Uiso/Uaniso restraints and constraints
O49 \\sim O0AA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O8 \\sim O3AA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O19 \\sim O16: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O1AA \\sim O3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O16 \\sim O19: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Zr1 \\sim Zr4 \\sim Zr6 \\sim Zr5 \\sim Zr2 \\sim Zr3: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C12 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C23 \\sim C24 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C97: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C96 \\sim C95 \\sim C94 \\sim C93 \\sim C92 \\sim C91: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C82 \\sim C83 \\sim C84 \\sim C79 \\sim C80 \\sim C81: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C71 \\sim C76 \\sim C75 \\sim C74 \\sim C73 \\sim C72: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C69 \\sim C70 \\sim C65 \\sim C66 \\sim C67 \\sim C68: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C63 \\sim C64 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C56 \\sim C57 \\sim C58 \\sim C53 \\sim C54 \\sim C55: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C32 \\sim C31 \\sim C30 \\sim C29 \\sim C28 \\sim C27: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C38 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C44 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C49 \\sim C50 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C88 \\sim C89 \\sim C90 \\sim C85 \\sim C86 \\sim C87: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C01 \\sim C1: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O49 \\sim O0AA \\sim C77: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O55 \\sim O17: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O5AA \\sim O4AA: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O19 \\sim C2AA \\sim O16: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
O1AA \\sim C0AA \\sim O3: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
O3AA \\sim O8 \\sim C51: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C77 \\sim O49 \\sim O0AA: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
O102 \\sim O7 \\sim O14 \\sim O23 \\sim O24 \\sim O27 \\sim O18 \\sim O28:
within 2A with sigma of 0.025 and sigma for terminal atoms of 0.05
O46 \\sim O88: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Zr3) \\sim Ueq, Uanis(Zr4) \\sim Ueq, Uanis(Zr6) \\sim Ueq, Uanis(Zr2)
\\sim Ueq, Uanis(Zr5) \\sim Ueq, Uanis(Zr1) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.01
Uanis(O49) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O42)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Zr5) \\sim Ueq, Uanis(Zr2) \\sim Ueq, Uanis(Zr1) \\sim Ueq, Uanis(Zr4)
\\sim Ueq, Uanis(Zr6) \\sim Ueq, Uanis(Zr3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O102) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O28) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O55) \\sim Ueq, Uanis(O2AA) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O17)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O88) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O88) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C94) \\sim Ueq,
Uanis(C93) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C102)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C98)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C01) \\sim Ueq, Uanis(O4AA) \\sim Ueq, Uanis(O5AA)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(O42) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(N5) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C70) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C72) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O55)
\\sim Ueq, Uanis(O2AA) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(O3AA) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O46) \\sim Ueq, Uanis(O4AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C01)
\\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O5AA) \\sim Ueq, Uanis(O42) \\sim Ueq,
Uanis(O2AA) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(N7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N5) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C87) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C34) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C91) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C69) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C97) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C99)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C73) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C2AA)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(O16) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1AA)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(O0AA) \\sim Ueq,
Uanis(O49) \\sim Ueq, Uanis(O3AA) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C1AA) \\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O88) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.01
8. Others
 Fixed Uiso: H1(0.13) H2(0.13) H3(0.13) H4(0.13) H5(0.13) H6(0.13) H7(0.13)
 H8(0.13) H2A(0.13) H3A(0.13) H5A(0.13) H6A(0.13) H8A(0.13) H9(0.13) H12(0.13)
 H14(0.13) H15(0.13) H17(0.13) H18(0.13) H20(0.13) H21(0.13) H23(0.13)
 H24(0.13) H28(0.13) H29(0.13) H31(0.13) H32(0.13) H34(0.13) H35(0.13)
 H37(0.13) H38(0.13) H40(0.13) H41(0.13) H43(0.13) H44(0.13) H46(0.13)
 H47(0.13) H49(0.13) H50(0.13) H54(0.13) H55(0.13) H57(0.13) H58(0.13)
 H60(0.13) H61(0.13) H63(0.13) H64(0.13) H66(0.13) H67(0.13) H69(0.13)
 H70(0.13) H72(0.13) H73(0.13) H75(0.13) H76(0.13) H80(0.13) H81(0.13)
 H83(0.13) H84(0.13) H86(0.13) H87(0.13) H89(0.13) H90(0.13) H92(0.13)
 H93(0.13) H95(0.13) H96(0.13) H98(0.13) H99(0.13) H101(0.13) H102(0.13)
 O1(0.08) O2(0.08)
 Fixed X: H17A(0.721961) H17B(0.66913) H2AA(0.88692) H2AB(0.936929)
 H21A(1.00533) H21B(1.05991) H55A(0.598821) H55B(0.55239) O1(0.721881)
 H1A(0.69248) H1B(0.750589) O2(0.72203) H2B(0.753901) H2C(0.693991)
 Fixed Y: H17A(0.28899) H17B(0.28732) H2AA(0.27098) H2AB(0.25212)
 H21A(0.305341) H21B(0.276389) H55A(0.27896) H55B(0.30092) O1(1.02795)
 H1A(1.01762) H1B(1.00161) O2(0.52696) H2B(0.539229) H2C(0.55361)
 Fixed Z: H17A(1.05343) H17B(1.00085) H2AA(1.055281) H2AB(1.00013)
 H21A(0.94224) H21B(0.899261) H55A(0.910749) H55B(0.85989) O1(1.28558)
 H1A(1.25181) H1B(1.292) O2(1.27599) H2B(1.254829) H2C(1.276179)
9.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), C2(H2A),
 C3(H3A), C5(H5A), C6(H6A), C8(H8A), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C28(H28),
  C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50),
  C54(H54), C55(H55), C57(H57), C58(H58), C60(H60), C61(H61), C63(H63),
 C64(H64), C66(H66), C67(H67), C69(H69), C70(H70), C72(H72), C73(H73), C75(H75),
  C76(H76), C80(H80), C81(H81), C83(H83), C84(H84), C86(H86), C87(H87),
 C89(H89), C90(H90), C92(H92), C93(H93), C95(H95), C96(H96), C98(H98), C99(H99),
  C101(H101), C102(H102)
9.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C8,C9,C10,C11,C12), C13(C14,C15,C16,C17,C18), C19(C20,
 C21,C22,C23,C24), C27(C28,C29,C30,C31,C32), C33(C34,C35,C36,C37,C38), C39(C40,
 C41,C42,C43,C44), C45(C46,C47,C48,C49,C50), C53(C54,C55,C56,C57,C58), C59(C60,
 C61,C62,C63,C64), C65(C66,C67,C68,C69,C70), C71(C72,C73,C74,C75,C76), C79(C80,
 C81,C82,C83,C84), C85(C86,C87,C88,C89,C90), C91(C92,C93,C94,C95,C96), C97(C98,
 C99,C100,C101,C102)
;
_shelx_res_checksum              83218
_shelx_fab_checksum              40869
_olex2_submission_special_instructions 'No special instructions were received'