Sterics and metal-ion radius control the self-assembly of [M2L3] helicates
Siddique, Rashid G.; Arachchige, Kasun; AL-Fayaad, Hydar; McMurtrie, John C.; Clegg, Jack Kay; Dalton Transactions  (2022) –; doi:10.1039/D2DT02241A

data_7710912
_publ_section_title
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 Sterics and metal-ion radius control the self-assembly of [M2L3]
 helicates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02241A
_journal_year                    2022
_chemical_formula_moiety         'C90 H54 N12 Zn2, 4[ClO4], 7.5[CH3CN], 6[H2O]'
_chemical_formula_sum            'C105 H88.5 N19.5 O22 Zn2'
_chemical_formula_weight         2248.49
_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     dual
_audit_creation_date             2021-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-02 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.67(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.060(6)
_cell_length_b                   15.235(3)
_cell_length_c                   45.929(9)
_cell_measurement_reflns_used    311386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.097
_cell_volume                     22432(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            275661
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.220
_diffrn_reflns_theta_max         25.220
_diffrn_reflns_theta_min         2.040
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             9276
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   26.372
_exptl_transmission_factor_min   1.097
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1873
_refine_ls_number_reflns         37610
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.1482
_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          0.3990
_refine_ls_wR_factor_ref         0.4126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28889
_reflns_number_total             37610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02241a2.cif
_cod_data_source_block           p21c_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C210 H178 Cl8 N39 O44 Zn4'
_cod_original_formula_weight         4496.98
_cod_original_formula_units_Z            4
_cod_database_code               7710912
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.00005
3.a Aromatic/amide H refined with riding coordinates:
 C167(H167), C27(H27), C100(H100), C23(H23), C70(H70), C143(H143), C78(H78),
 C40(H40), C157(H157), C158(H158), C160(H160), C37(H37), C24(H24), C22(H22),
 C83(H83), C144(H144), C17(H17), C172(H172), C135(H135), C75(H75), C84(H84),
 C62(H62), C53(H53), C7(H7), C52(H52), C112(H112), C31(H31), C114(H114),
 C107(H107), C38(H38), C32(H32), C102(H102), C61(H61), C68(H68), C54(H54),
 C94(H94), C12(H12), C45(H45), C162(H162), C113(H113), C64(H64), C82(H82),
 C147(H147), C91(H91), C67(H67), C142(H142), C98(H98), C127(H127), C97(H97),
 C10(H10), C150(H150), C4(H4), C63(H63), C130(H130), C138(H138), C8(H8),
 C120(H120), C48(H48), C0AA(H0AA), C92(H92), C128(H128), C173(H173), C90(H90),
 C154(H154), C28(H28), C149(H149), C151(H151), C152(H152), C119(H119), C60(H60),
  C148(H148), C177(H177), C124(H124), C1(H1), C34(H34), C174(H174), C123(H123),
 C59(H59), C93(H93), C57(H57), C33(H33), C118(H118), C2(H2), C121(H121),
 C153(H153), C30(H30), C3(H3), C89(H89), C58(H58), C122(H122), C87(H87),
 C117(H117), C180(H180), C179(H179), C88(H88), C178(H178)
3.b :
 C110(H110), C165(H165), C170(H170), C80(H80), C15(H15), C74(H74), C105(H105),
 C44(H44), C134(H134), C140(H140), C20(H20), C50(H50)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 3366 electrons were 
found in a volume of 11111\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
8[ClO4], 15[CH3CN], 12[H2O] per Asymmetric Unit 
which account for 2888 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8454
_shelx_hkl_checksum              94419
_shelx_fab_checksum              27459
_olex2_submission_special_instructions 'No special instructions were received'