Supramolecular Isomorphic Dodecanuclear Cobalt Clusters with Same Metal Shell but Different Core Ligands
Liang, Xiao-Wen; Zhang, Lin-Lin; Zhang, Ting; Zhao, Jiong-Peng; liu, fuchen; Dalton Transactions  (2022) –; doi:10.1039/D2DT00915C

data_7710166
_publ_section_title
;
 Supramolecular Isomorphic Dodecanuclear Cobalt Clusters with Same Metal
 Shell but Different Core Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00915C
_journal_year                    2022
_chemical_formula_moiety         'C128 H97 Co12 N29 O21, 4(OH)'
_chemical_formula_sum            'C128 H101 Co12 N29 O25'
_chemical_formula_weight         3152.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                101.341(6)
_cell_angle_beta                 96.206(5)
_cell_angle_gamma                101.395(7)
_cell_formula_units_Z            2
_cell_length_a                   17.2087(14)
_cell_length_b                   17.2439(15)
_cell_length_c                   27.3335(15)
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3980
_cell_measurement_theta_min      2.7240
_cell_volume                     7704.3(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     85.00 111.00   1.00   27.50    --   30.00  54.00-150.00   26
  2  \w    -73.00  36.00   1.00   27.50    --   30.00  54.00 -30.00  109
  3  \w    -73.00  32.00   1.00   27.50    --   30.00  54.00  90.00  105
  4  \w    -73.00  32.00   1.00   27.50    --   30.00  54.00-150.00  105
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0257484000
_diffrn_orient_matrix_UB_12      -0.0392185000
_diffrn_orient_matrix_UB_13      -0.0074729000
_diffrn_orient_matrix_UB_21      0.0129757000
_diffrn_orient_matrix_UB_22      -0.0083743000
_diffrn_orient_matrix_UB_23      0.0235449000
_diffrn_orient_matrix_UB_31      -0.0312869000
_diffrn_orient_matrix_UB_32      0.0156594000
_diffrn_orient_matrix_UB_33      0.0103463000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.1507
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42666
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1764
_refine_ls_number_reflns         27135
_refine_ls_number_restraints     4381
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0893P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13965
_reflns_number_total             27135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00915c2.cif
_cod_data_source_block           2
_cod_original_cell_volume        7704.3(10)
_cod_database_code               7710166
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Restrained distances
 C68A-C67 = C68B-C67
 1.5 with sigma of 0.01
 N23-N24 \\sim N24-N25
 with sigma of 0.02
 N25-N24 \\sim N24-N23
 with sigma of 0.02
 C68B-C67 \\sim C68A-C67
 with sigma of 0.02
 O2-N1 \\sim O1-N1 \\sim O3-N1 \\sim O4-N2 \\sim O5-N2 \\sim O6-N2
 with sigma of 0.01
 N20-N19 \\sim N27-N26 \\sim N28-N26 \\sim N29-N27 \\sim N21-N19 \\sim N22-N20
\\sim N16-N15 \\sim N17-N15
 \\sim N18-N16
 with sigma of 0.01
2. Rigid bond restraints
 N23, N24, N27, N29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N25, N24, N23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N25, N24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68B, C67, C68A, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, N1, O1, N1, O3, N1, O4, N2, O5, N2, O6, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N20, N19, N27, N26, N28, N26, N29, N27, N21, N19, N22, N20, N16, N15, N17,
 N15, N18, N16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Co3, Co9, O20, O21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N24 \\sim N23 \\sim N25: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03 within 3.8A
N25 \\sim N24: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.08 within 3.8A
C68B \\sim C68A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.03 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O25 \\sim O22 \\sim O24 \\sim O23
\\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C65 \\sim C66 \\sim C67 \\sim C68A \\sim C69 \\sim C70 \\sim C71 \\sim C72
\\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80
\\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88
\\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96
\\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C104 \\sim
C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim
C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118 \\sim
C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim
C126 \\sim C127 \\sim C128 \\sim C129 \\sim C68B: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03 within 3.8A
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C68B)
\\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 N23, N24, N25, Co11, Co5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N25, N24, N23, Co11, Co5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C68A(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C68B(0.5) H68D(0.5)
 H68E(0.5) H68F(0.5)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C30(H30), C50(H50), C78(H78), C98(H98), C119(H119)
6.b Me refined with riding coordinates:
 C62(H62A,H62B,H62C), C68A(H68A,H68B,H68C), C68B(H68D,H68E,H68F)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C13(H13), C14(H14), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C33(H33),
  C34(H34), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
 C45(H45), C46(H46), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60), C69(H69),
  C70(H70), C71(H71), C76(H76), C77(H77), C81(H81), C82(H82), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C96(H96), C97(H97),
 C101(H101), C104(H104), C107(H107), C108(H108), C109(H109), C110(H110),
 C111(H111), C112(H112), C117(H117), C118(H118), C123(H123), C124(H124),
 C126(H126), C128(H128), C129(H129)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C51(H51A,H51B,H51C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C), C79(H79A,H79B,H79C), C99(H99A,H99B,H99C),
 C120(H12A,H12B,H12C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 275 electrons were 
found in a volume of 2189\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[C2H5OH], 0.5[H2O] per Formula Unit 
which account for 270 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92713
_shelx_fab_checksum              5313
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.721