Synthesis, polymorphism, and shape complementarity-induced co-crystallization of hexanuclear Co(II) clusters capped by a flexible heteroligand shell.
Terlecki, Michał; Kornowicz, Arkadiusz; Sacharczuk, Kornel; Justyniak, Iwona; Lewiński, Janusz; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7012–7022; doi:10.1039/d4dt00261j

data_7715569
_publ_section_title
;
 Synthesis, polymorphism, and shape complementarity-induced
 co-crystallization of hexanuclear Co(II) clusters capped by a flexible
 heteroligand shell.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7012
_journal_page_last               7022
_journal_paper_doi               10.1039/d4dt00261j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C48 H90 Co6 N6 O18'
_chemical_formula_sum            'C48 H90 Co6 N6 O18'
_chemical_formula_weight         1392.83
_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
_audit_creation_date             2024-03-19
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.439(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2702(2)
_cell_length_b                   13.7088(3)
_cell_length_c                   17.3126(3)
_cell_measurement_reflns_used    7254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1500
_cell_measurement_theta_min      2.9087
_cell_volume                     2911.23(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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 (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15030
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.214
_diffrn_reflns_theta_min         2.972
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet-pink
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+4.8058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5973
_reflns_number_total             6780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00261j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715569--7715573.cif.'
_cod_database_code               7715569
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C20 \\sim C20A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002 within 2A
3. Others
 Sof(H19C)=Sof(H19D)=Sof(H21C)=Sof(H21D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(H21A)=Sof(H21B)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C19(H19C,
 H19D), C21(H21A,H21B), C21(H21C,H21D), C22(H22A,H22B), C20(H20A,H20B),
 C20A(H20C,H20D)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              5556
_olex2_submission_special_instructions 'No special instructions were received'