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_7710913
_publ_section_title
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 Sterics and metal-ion radius control the self-assembly of [M2L3]
 helicates
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02241A
_journal_year                    2022
_chemical_formula_moiety         'C90 H54 Co2 N12, 4[C2H3N], 4[ClO4]'
_chemical_formula_sum            'C98 H66 Cl4 Co2 N16 O16'
_chemical_formula_weight         1983.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.876(3)
_cell_length_b                   40.319(8)
_cell_length_c                   33.407(7)
_cell_measurement_reflns_used    16797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.219
_cell_measurement_theta_min      2.089
_cell_volume                     18690(7)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            199521
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.219
_diffrn_reflns_theta_max         25.219
_diffrn_reflns_theta_min         2.089
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       cube
_exptl_crystal_F_000             8128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0
_exptl_transmission_factor_min   0
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         16797
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.2101
_refine_ls_R_factor_gt           0.1468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+95.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3449
_refine_ls_wR_factor_ref         0.3880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6920
_reflns_number_total             16797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02241a2.cif
_cod_data_source_block           pbcn_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 
;
_cod_database_code               7710913
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C33-C34
 1.45 with sigma of 0.02
 C75-C72
 1.45 with sigma of 0.02
 C19-C20
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.0005
Uanis(N10) = Uanis(C86) = Uanis(C87) = Uanis(C88) = Uanis(C90) = Uanis(C89)
Uanis(C27) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) =
Uanis(N4)
Uanis(C15) = Uanis(C14)
4.a Aromatic/amide H refined with riding coordinates:
 C55(H55), C50(H50), C45(H45), C85(H85), C70(H70), C67(H67), C12(H12),
 C22(H22), C80(H80), C38(H38), C10(H10), C52(H52), C64(H64), C7(H7), C40(H40),
 C68(H68), C82(H82), C87(H87), C88(H88), C89(H89), C90(H90), C83(H83), C2(H2),
 C17(H17), C53(H53), C37(H37), C3(H3), C60(H60), C75(H75), C63(H63), C61(H61),
 C1(H1), C8(H8), C62(H62), C31(H31), C27(H27), C25(H25), C34(H34), C4(H4),
 C24(H24), C28(H28), C29(H29), C30(H30), C59(H59), C32(H32), C57(H57), C33(H33),
  C58(H58)
4.b Fitted hexagon refined as free rotating group:
 C86(C87,C88,C89,C90,N10)
4.c :
 C49(H49), C44(H44), C79(H79), C20(H20), C15(H15), C74(H74)
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_smtbx_masks_special_details
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A solvent mask was calculated and 2444 electrons were 
found in a volume of 6984\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4.0[C2H3N], 4[ClO4] per Asymmetric Unit 
which account for 2272 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11947
_shelx_hkl_checksum              84611
_shelx_fab_checksum              85667
_olex2_submission_special_instructions 'No special instructions were received'