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_7715572
_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         'C44 H86 Co6 N6 O16'
_chemical_formula_sum            'C44 H86 Co6 N6 O16'
_chemical_formula_weight         1308.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-03-21
_audit_creation_method
;
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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6327(3)
_cell_length_b                   15.3660(3)
_cell_length_c                   27.9274(5)
_cell_measurement_reflns_used    7136
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.0703
_cell_measurement_theta_min      3.0181
_cell_volume                     5421.10(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
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 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -93.00  -54.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4221  165.0000  -73.0000 39

  2 omega   45.00   82.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0002  178.0000   60.0000 37

  3 omega   55.00   82.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0002   57.0000  -90.0000 27

  4 omega   59.00   86.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0002  178.0000 -180.0000 27

  5 omega  -20.00   28.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0002  -99.0000 -120.0000 48

  6 omega   21.00   48.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0002  -77.0000  116.0000 27
;
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19815
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.024
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.800
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       plate
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         10589
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0340P)^2^+2.8434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.833
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                9147
_reflns_number_total             10589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00261j2.cif
_cod_data_source_block           1gamma
_cod_depositor_comments
'Adding full bibliography for 7715569--7715573.cif.'
_cod_database_code               7715572
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.73(2)
 0.27(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O6-H6
 0.98 with sigma of 0.001
 O12-H12
 0.98 with sigma of 0.001
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), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              83512
_olex2_submission_special_instructions 'No special instructions were received'