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_7233981
_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
'C82.25 H64.25 N7.5 O14.47 Zn4, 4(C3 H7 N O), 0.5(C6 H14 N2 O)'
_chemical_formula_sum            'C97.25 H99.25 N12.5 O18.96 Zn4'
_chemical_formula_weight         2007.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                101.926(3)
_cell_angle_beta                 96.440(3)
_cell_angle_gamma                98.138(3)
_cell_formula_units_Z            2
_cell_length_a                   15.2047(6)
_cell_length_b                   18.4315(6)
_cell_length_c                   28.6082(11)
_cell_measurement_reflns_used    20132
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.02
_cell_measurement_theta_min      2.12
_cell_volume                     7682.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
_diffrn_measurement_method       'rotanting crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            98855
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.944
_diffrn_reflns_theta_min         1.472
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_type   multi-scan
_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    0.868
_exptl_crystal_description       plate
_exptl_crystal_F_000             2084
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         28924
_refine_ls_number_restraints     1331
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.1291
_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          0.3141
_refine_ls_wR_factor_ref         0.3374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19085
_reflns_number_total             28924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01230c2.cif
_cod_data_source_block           znflexlp
_cod_depositor_comments
'Adding full bibliography for 7233980--7233983.cif.'
_cod_original_cell_volume        7682.0(5)
_cod_original_formula_sum        'C97.25 H99.25 N12.50 O18.96 Zn4'
_cod_database_code               7233981
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C27
 1.494 with sigma of 0.02
 C92B-N12
 1.468 with sigma of 0.02
 N12-C91B
 1.455 with sigma of 0.02
 O19S-C90B
 1.197 with sigma of 0.02
 N12-C90B
 1.351 with sigma of 0.02
 C90A-N2A
 1.343 with sigma of 0.02
 O20S-C93B
 1.21 with sigma of 0.02
 C93B-N1AA
 1.363 with sigma of 0.02
 N1AA-C95B
 1.453 with sigma of 0.02
 N1AA-C91A
 1.461 with sigma of 0.02
 C95B-N2A
 1.461 with sigma of 0.02
 N2A-C13A
 1.461 with sigma of 0.02
 C92A-N1AA
 1.461 with sigma of 0.02
 N1AA-C93B
 1.351 with sigma of 0.02
 O6-O7
 2.223 with sigma of 0.04
 C88-C89
 2.55 with sigma of 0.04
 C91B-C92B
 2.447 with sigma of 0.04
 N12-O19S
 2.249 with sigma of 0.04
 C90B-C91B
 2.55 with sigma of 0.04
 C92B-C91B
 2.55 with sigma of 0.04
 C95B-C91A
 2.49 with sigma of 0.04
 C95B-C93B
 2.446 with sigma of 0.04
 O20S-N1AA
 2.298 with sigma of 0.04
 C95B-C13A
 2.45 with sigma of 0.04
 C92A-C93B
 2.4 with sigma of 0.04
 C93B-C91A
 2.506 with sigma of 0.04
 C57B-C56B \\sim C57A-C56A
 with sigma of 0.02
 C57B-C58B \\sim C57A-C58A
 with sigma of 0.02
 C56B-C55B \\sim C56A-C55A
 with sigma of 0.02
 C55B-C54B \\sim C55A-C54A
 with sigma of 0.02
 C54B-C59B \\sim C54A-C59A
 with sigma of 0.02
 C59B-C58B \\sim C59A-C58A
 with sigma of 0.02
 C57B-C55B \\sim C57A-C55A
 with sigma of 0.04
 C57B-C59B \\sim C57A-C59A
 with sigma of 0.04
 C56B-C54B \\sim C56A-C54A
 with sigma of 0.04
 C56B-C58B \\sim C56A-C58A
 with sigma of 0.04
 C55B-C59B \\sim C55A-C59A
 with sigma of 0.04
 C54B-C58B \\sim C54A-C58A
 with sigma of 0.04
 N12-C90B \\sim N12A-C4AA
 with sigma of 0.02
 O19S-C90B \\sim O19S-C4AA
 with sigma of 0.02
 N12-O19S \\sim N12A-O19S
 with sigma of 0.04
 O20S-C93B \\sim O21S-C90A
 with sigma of 0.02
 C93B-N1AA \\sim C90A-N2A
 with sigma of 0.02
 N1AA-C95B \\sim N2A-C92A
 with sigma of 0.02
 N1AA-C91A \\sim N2A-C13A
 with sigma of 0.02
 O20S-N1AA \\sim O21S-N2A
 with sigma of 0.04
 C93B-C95B \\sim C90A-C92A
 with sigma of 0.04
 C93B-C91A \\sim C90A-C13A
 with sigma of 0.04
 C95B-C91A \\sim C92A-C13A
 with sigma of 0.04
 C66-C63A \\sim C66-C63B
 with sigma of 0.02
 C65A-C60A \\sim C61B-C60B
 with sigma of 0.02
 C65A-C64A \\sim C61B-C62B
 with sigma of 0.02
 C60A-C61A \\sim C60B-C65B
 with sigma of 0.02
 C61A-C62A \\sim C65B-C64B
 with sigma of 0.02
 C62A-C63A \\sim C64B-C63B
 with sigma of 0.02
 C63A-C64A \\sim C63B-C62B
 with sigma of 0.02
 C66-C62A \\sim C66-C64B
 with sigma of 0.04
 C66-C64A \\sim C66-C62B
 with sigma of 0.04
 C65A-C61A \\sim C61B-C65B
 with sigma of 0.04
 C65A-C63A \\sim C61B-C63B
 with sigma of 0.04
 C60A-C62A \\sim C60B-C64B
 with sigma of 0.04
 C60A-C64A \\sim C60B-C62B
 with sigma of 0.04
 C61A-C63A \\sim C65B-C63B
 with sigma of 0.04
 C62A-C64A \\sim C64B-C62B
 with sigma of 0.04
 N5A-C60A \\sim N5A-C60B
 with sigma of 0.02
 N5B-C60A \\sim N5B-C60B
 with sigma of 0.02
 N5A-C65A \\sim N5A-C61B
 with sigma of 0.04
 N5A-C61A \\sim N5A-C65B
 with sigma of 0.04
 N5B-C65A \\sim N5B-C61B
 with sigma of 0.04
 N5B-C61A \\sim N5B-C65B
 with sigma of 0.04
 N12-C92B \\sim N12A-C6AA
 with sigma of 0.02
 N12-C91B \\sim N12A-C5AA
 with sigma of 0.02
 C90B-C92B \\sim C4AA-C6AA
 with sigma of 0.04
 C90B-C91B \\sim C4AA-C5AA
 with sigma of 0.04
 C92B-C91B \\sim C6AA-C5AA
 with sigma of 0.04
3. Restrained planarity
 C56A, C57A, C58A, C59A, C54A, C55A, N5A
 with sigma of 0.1
 C57B, C56B, C55B, C54B, C59B, C58B, N5A
 with sigma of 0.1
 C53B, C54B, C55B, C59B, C58B, C57B, N5B, C56B
 with sigma of 0.1
 C90B, N12, C92B, C91B, O19S
 with sigma of 0.1
 O20S, C93B, N1AA, C91A, C92A
 with sigma of 0.1
 C91B, C90B, C92B, N12, O19S
 with sigma of 0.1
 C95B, N2A, C13A, C90A, O21S
 with sigma of 0.1
 C66, C67, C71, C63A, C60A
 with sigma of 0.1
 C6AA, C5AA, N12A, C4AA
 with sigma of 0.1
4. Rigid bond restraints
 C12, C11, C10, C9, C8, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C25, C24, C23, C22, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C31, C30, C29, C28, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, C40, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C50, C49, C48, C47, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1AA, C0AA, C74, C73, C72, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C71, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O17S, C81, N9S, C82, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C83, N9S, C81, O17S, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57B, C56B, C55B, C54B, C59B, C58B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57A, C58A, C59A, C54A, C55A, C56A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58B, C59B, C54B, C55B, C56B, C57B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, O7, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O11A, C53B, O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C79, C80
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C89, N0AA, C87, O18S, C88
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88, C89
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C92B, N12, C90B, O19S, C91B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C91B, C92B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C90B, N12, C92B, C91B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C93B, N1AA, C95B, C91A, O20S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C95B, N1AA, C91A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C95B, C91A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13A, C95B, N2A, C90A, O21S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C93B, O20S, N1AA, C91A, C92A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C95B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55A, C54A, C59A, C58A, C57A, C56A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59A, C58A, C57A, C56A, C55A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66, C71, C70, C69, C68, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C72, C2AA, C1AA, C0AA, C74, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61A, C60A, C65A, C64A, C63A, C62A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C60A, C61A, C62A, C63A, C64A, C65A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C90B, O19S, N12, C91B, C92B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C92A, N1AA, C93B, O20S, C91A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6AA, N12A, C4AA, C5AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6AA, N12A, C5AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C46: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C44 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C45: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C35 \\sim C34 \\sim C39 \\sim C38 \\sim C37 \\sim C36: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C32 \\sim C31 \\sim C30 \\sim C29 \\sim C28 \\sim C33: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C2AA \\sim C1AA \\sim C0AA \\sim C74 \\sim C73 \\sim C72: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C6 \\sim C7 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C13 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C67 \\sim C66 \\sim C71 \\sim C70 \\sim C69 \\sim C68: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C58B \\sim C59B \\sim C54B \\sim C55B \\sim C56B \\sim C57B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C58A \\sim C57A \\sim C56A \\sim C55A \\sim C54A \\sim C59A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O11A \\sim C53B \\sim O10: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C80 \\sim C79: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C87 \\sim O18S \\sim N0AA \\sim C89 \\sim C88: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C89 \\sim C88: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C90B \\sim O19S \\sim N12 \\sim C92B \\sim C91B: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C93B \\sim N1AA \\sim C95B \\sim C91A \\sim O20S: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
O20S \\sim C93B \\sim N1AA \\sim C91A \\sim C92A \\sim C95B \\sim N2A \\sim
C90A \\sim C13A \\sim O21S: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C64B \\sim C63B \\sim C62B \\sim C61B \\sim C60B \\sim C65B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim N5A: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N5B \\sim C60A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C90B \\sim N12 \\sim C92B \\sim C91B \\sim O19S: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C90B \\sim N12 \\sim C92B \\sim C91B \\sim O19S \\sim C4AA \\sim N12A \\sim
C5AA \\sim C6AA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C6AA \\sim C5AA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C79) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C80)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C78) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.1
Uanis(C79) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N5B) \\sim Ueq, Uanis(N5A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.05
Uanis(C65B) \\sim Ueq, Uanis(C64B) \\sim Ueq, Uanis(C63B) \\sim Ueq,
Uanis(C62B) \\sim Ueq, Uanis(C61B) \\sim Ueq, Uanis(C60B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.05
Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(N0AA) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(O18S) \\sim Ueq: with sigma of 0.025 and sigma for terminal
atoms of 0.05
Uanis(C13A) \\sim Ueq, Uanis(C95B) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C90A)
\\sim Ueq, Uanis(O21S) \\sim Ueq: with sigma of 0.1 and sigma for terminal
atoms of 0.2
Uanis(C92A) \\sim Ueq, Uanis(O20S) \\sim Ueq, Uanis(C93B) \\sim Ueq,
Uanis(N1AA) \\sim Ueq, Uanis(C91A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(N2A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C95B) \\sim Ueq, Uanis(C90A)
\\sim Ueq, Uanis(O21S) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C92B) \\sim Ueq, Uanis(C91B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C64B) \\sim Ueq, Uanis(C63B) \\sim Ueq, Uanis(C62B) \\sim Ueq,
Uanis(C61B) \\sim Ueq, Uanis(C60B) \\sim Ueq, Uanis(C65B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54A) \\sim Ueq, Uanis(C59A) \\sim Ueq, Uanis(C55A) \\sim Ueq,
Uanis(C56A) \\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(N5A)
\\sim Ueq, Uanis(N5B) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C60A) \\sim Ueq,
Uanis(C61A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C63A) \\sim Ueq,
Uanis(C64A) \\sim Ueq, Uanis(C62B) \\sim Ueq, Uanis(C61B) \\sim Ueq,
Uanis(C60B) \\sim Ueq, Uanis(C65B) \\sim Ueq, Uanis(C64B) \\sim Ueq,
Uanis(C63B) \\sim Ueq, Uanis(C58B) \\sim Ueq, Uanis(C57B) \\sim Ueq,
Uanis(C56B) \\sim Ueq, Uanis(C55B) \\sim Ueq, Uanis(C54B) \\sim Ueq,
Uanis(C59B) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C61A) \\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(C65A) \\sim Ueq,
Uanis(C64A) \\sim Ueq, Uanis(C63A) \\sim Ueq, Uanis(C62A) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C4AA) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C90B) \\sim Ueq, Uanis(C92B)
\\sim Ueq, Uanis(C91B) \\sim Ueq, Uanis(O19S) \\sim Ueq, Uanis(N12A) \\sim Ueq,
Uanis(C5AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
6. Others
 Fixed Sof: C58B(0.5) H58B(0.5) C57B(0.5) C56B(0.5) H56B(0.5) C55B(0.5)
 H55B(0.5) C54B(0.5) C59B(0.5) H59B(0.5) C56A(0.5) H56A(0.5) C55A(0.5)
 H55A(0.5) C54A(0.5) C59A(0.5) H59A(0.5) C58A(0.5) H58A(0.5) C57A(0.5) N5A(0.5)
 H5A(0.5) N5B(0.5) H5B(0.5) C61A(0.5) H61A(0.5) C62A(0.5) H62A(0.5) C63A(0.5)
 C64A(0.5) H64A(0.5) C65A(0.5) H65A(0.5) C60A(0.5) C62B(0.5) H62B(0.5)
 C61B(0.5) H61B(0.5) C60B(0.5) C65B(0.5) H65B(0.5) C64B(0.5) H64B(0.5)
 C63B(0.5) C53B(0.5) O11A(0.5) O14(0.5) C78(0.5) H78(0.5) N8(0.5) C80(0.5)
 H80A(0.5) H80B(0.5) H80C(0.5) C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5) C75(0.75)
 H75(0.75) O20S(0.5) C93B(0.5) H93B(0.5) N1AA(0.5) C95B(0.5) H95A(0.5)
 H95B(0.5) H95C(0.5) C91A(0.5) H91D(0.5) H91E(0.5) H91F(0.5) N12(0.5) O19S(0.5)
 C90B(0.5) H90B(0.5) C92B(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C91B(0.5)
 H91A(0.5) H91B(0.5) H91C(0.5) C53A(0.5) C4AA(0.5) H4AA(0.5) C5AA(0.5)
 H5AA(0.5) H5AB(0.5) H5AC(0.5) N12A(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5)
 H6AC(0.5) O21S(0.5) C90A(0.5) H90A(0.5) N2A(0.5) C92A(0.5) H92D(0.5) H92E(0.5)
 H92F(0.5) C13A(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 Fixed X: H95A(0.47878) H95B(0.38421) H95C(0.41494) H91D(0.51344)
 H91E(0.48897) H91F(0.58228) H89A(-0.10907) H89B(-0.20784) H89C(-0.1304) H92A(-
 0.0081) H92B(-0.04183) H92C(0.059669) H91A(-0.147659) H91B(-0.128551) H91C(-
 0.09889) H5AA(-0.12746) H5AB(-0.08588) H5AC(-0.081511) H6AA(0.09795)
 H6AB(0.0022) H6AC(0.02458) H92D(0.404699) H92E(0.37331) H92F(0.350841)
 H13A(0.536109) H13B(0.43112) H13C(0.48364)
 Fixed Y: H95A(-0.17532) H95B(-0.213971) H95C(-0.12706) H91D(-0.27605) H91E(-
 0.29125) H91F(-0.24414) H89A(-0.099951) H89B(-0.08566) H89C(-0.041511)
 H92A(0.51946) H92B(0.43314) H92C(0.46281) H91A(0.42158) H91B(0.42768)
 H91C(0.36231) H5AA(0.48884) H5AB(0.510961) H5AC(0.57197) H6AA(0.45237)
 H6AB(0.430749) H6AC(0.393861) H92D(-0.13153) H92E(-0.21896) H92F(-0.17048)
 H13A(-0.271199) H13B(-0.292581) H13C(-0.29185)
 Fixed Z: H95A(0.02961) H95B(0.036909) H95C(0.056589) H91D(0.118961)
 H91E(0.06269) H91F(0.08827) H89A(-0.334029) H89B(-0.34445) H89C(-0.364639)
 H92A(0.14487) H92B(0.12409) H92C(0.14502) H91A(0.169861) H91B(0.22566)
 H91C(0.18973) H5AA(0.169381) H5AB(0.12551) H5AC(0.17325) H6AA(0.14311)
 H6AB(0.11231) H6AC(0.155951) H92D(0.056829) H92E(0.04358) H92F(0.091181)
 H13A(0.114161) H13B(0.10559) H13C(0.06151)
7.a Free rotating group:
 O18S(C87,N0AA,C88,H88A,H88B,H88C)
7.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N2(H2), C30(H30), C29(H29), C33(H33), C32(H32), N4(H4),
 C21(H21), C25(H25), C24(H24), C22(H22), C45(H45), C44(H44), C42(H42), C41(H41),
  C6(H6), C4(H4A), C3(H3A), C7(H7), N6(H6A), C51(H51), C47(H47), C48(H48),
 C50(H50), C81(H81), C13(H13), C12(H12), C10(H10), C9(H9), C15(H15), C19(H19),
 C18(H18), C16(H16), C36(H36), C38(H38), C39(H39), C35(H35), C73(H73),
 C2AA(H2AA), C1AA(H1AA), C74(H74), C84(H84), C67(H67), C68(H68), C70(H70),
 C71(H71), C58B(H58B), C56B(H56B), C55B(H55B), C59B(H59B), C56A(H56A),
 C55A(H55A), C59A(H59A), C58A(H58A), N5A(H5A), N5B(H5B), C61A(H61A), C62A(H62A),
  C64A(H64A), C65A(H65A), C62B(H62B), C61B(H61B), C65B(H65B), C64B(H64B),
 C78(H78), C75(H75), C87(H87), C93B(H93B), C90B(H90B), C4AA(H4AA), C90A(H90A)
7.c Fitted hexagon refined as free rotating group:
 C30(C29,C28,C33,C32,C31), C21(C20,C25,C24,C23,C22), C45(C44,C43,C42,C41,C40),
 C6(C5,C4,C3,C2,C7), C51(C46,C47,C48,C49,C50), C13(C12,C11,C10,C9,C8), C15(C14,
 C19,C18,C17,C16), C36(C37,C38,C39,C34,C35), C73(C72,C2AA,C1AA,C0AA,C74),
 C67(C68,C69,C70,C71,C66), C58B(C57B,C56B,C55B,C54B,C59B), C56A(C55A,C54A,C59A,
 C58A,C57A), C61A(C62A,C63A,C64A,C65A,C60A), C62B(C61B,C60B,C65B,C64B,C63B)
7.d Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C80(H80A,H80B,H80C), C79(H79A,H79B,H79C), C77(H77A,H77B,H77C), C76(H76A,
 H76B,H76C)
;
_shelx_res_checksum              87831
_shelx_fab_checksum              13477
_olex2_exptl_crystal_mounting_method 'Solvotthermal synthesis'
_olex2_submission_special_instructions 'No special instructions were received'