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_7710165
_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         'C126 H94 Co12 N35 O19, 3(OH)'
_chemical_formula_sum            'C126 H97 Co12 N35 O22'
_chemical_formula_weight         3160.54
_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
_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                101.090(8)
_cell_angle_beta                 96.192(9)
_cell_angle_gamma                101.735(9)
_cell_formula_units_Z            2
_cell_length_a                   17.0982(19)
_cell_length_b                   17.2094(16)
_cell_length_c                   27.081(3)
_cell_measurement_reflns_used    3584
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.3870
_cell_measurement_theta_min      2.7440
_cell_volume                     7566.2(14)
_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    'ShelXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_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     18.00  45.00   1.00   62.50    --   30.00  54.00 150.00   27
  2  \w    -65.00 -38.00   1.00   62.50    --   30.00  54.00 -90.00   27
  3  \w     19.00 119.00   1.00   62.50    --   30.00  54.00 -90.00  100
  4  \w     66.00 115.00   1.00   62.50    --   30.00  54.00-150.00   49
  5  \w    -73.00 111.00   1.00   62.50    --   30.00  54.00  30.00  184
;
_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      0.0204809000
_diffrn_orient_matrix_UB_12      -0.0224767000
_diffrn_orient_matrix_UB_13      0.0141867000
_diffrn_orient_matrix_UB_21      0.0357268000
_diffrn_orient_matrix_UB_22      0.0133127000
_diffrn_orient_matrix_UB_23      -0.0100726000
_diffrn_orient_matrix_UB_31      0.0119300000
_diffrn_orient_matrix_UB_32      0.0343493000
_diffrn_orient_matrix_UB_33      0.0206568000
_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  0.1719
_diffrn_reflns_av_unetI/netI     0.3349
_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       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45285
_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         2.511
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12457
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1774
_refine_ls_number_reflns         26653
_refine_ls_number_restraints     6892
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.2204
_refine_ls_R_factor_gt           0.1029
_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^)+(0.0718P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2191
_refine_ls_wR_factor_ref         0.2959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8888
_reflns_number_total             26653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00915c2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7566.3(13)
_cod_database_code               7710165
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1. Restrained distances
 O22-O20
 2.8 with sigma of 0.1
 N33-N34 \\sim N33-N36 \\sim N35-N34 \\sim N35-N36
 with sigma of 0.02
2. Rigid bond restraints
 C16, C15, C13, C12, C14, C13, C6, C5, C9, C6, C12, C10, C17, C12, C15, C14,
 C5, C4, C9, C8, C9, C10, C57, C56, C57, C52, C56, C55, C60, C59, C20, C19, C66,
  C65, C11, C10, C17, C16, C18, C15, C29, C25, C29, C28, C2, C1, C22, C21, C25,
 C24, C64, C63, C4, C3, C7, C4, C8, C7, C127, C119, C127, C126, C112, C111,
 C113, C112, C52, C50, C53, C52, C55, C54, C58, C55, C59, C58, C19, C18, C28,
 C27, C30, C28, C3, C2, C23, C22, C24, C23, C26, C24, C119, C117, C120, C119,
 C126, C122, C116, C111, C114, C113, C117, C113, C46, C45, C47, C46, C50, C47,
 C51, C50, C54, C53, C40, C39, C40, C110, C38, C37, C39, C35, C42, C41, C45,
 C44, C62, C61, C27, C26, C31, C30, C30, C110, C75, C71, C75, C74, C125, C124,
 C68, C67, C71, C70, C118, C117, C121, C120, C122, C121, C123, C122, C95, C91,
 C95, C94, C88, C87, C91, C90, C108, C107, C116, C109, C116, C115, C115, C114,
 C48, C47, C33, C110, C37, C32, C35, C32, C35, C34, C43, C42, C44, C43, C49,
 C44, C74, C73, C76, C74, C124, C123, C69, C68, C70, C69, C72, C70, C94, C93,
 C96, C94, C89, C88, C90, C89, C92, C90, C109, C108, C49, C48, C79, C78, C83,
 C78, C34, C33, C99, C98, C99, C100, C73, C72, C77, C76, C79, C76, C83, C82,
 C85, C84, C101, C100, C106, C105, C93, C92, C97, C96, C98, C96, C80, C79, C98,
 C103, C82, C81, C86, C82, C86, C85, C102, C101, C104, C101, C105, C104, C81,
 C80, C103, C102
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N23 \\sim N24 \\sim N25 \\sim N30 \\sim N31 \\sim N32: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
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 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 C68 \\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 C103 \\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 N33 \\sim N35 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5
\\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim N10 \\sim N11 \\sim N12 \\sim N13
\\sim N14 \\sim N15 \\sim N16 \\sim N17 \\sim N18 \\sim N19 \\sim N20 \\sim N21
\\sim N22 \\sim N23 \\sim N24 \\sim N25 \\sim N26 \\sim N27 \\sim N28 \\sim N29
\\sim N30 \\sim N31 \\sim N32 \\sim N36 \\sim N34 \\sim 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 O22: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03 within 3.8A
N33 \\sim N35 \\sim N36 \\sim N34: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 2A
4. Others
 Fixed Sof: N36(0.5) N34(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C30(H30), C50(H50), C76(H76), C96(H96), C117(H117)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
 C48(H48), C49(H49), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60), C67(H67),
  C68(H68), C69(H69), C72(H72), C73(H73), C80(H80), C81(H81), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C92(H92), C93(H93),
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108), C109(H109), C114(H114), C115(H115), C120(H120), C121(H121),
 C123(H123), C124(H124), C125(H125)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C51(H51A,H51B,H51C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C77(H77A,H77B,H77C), C97(H97A,
 H97B,H97C), C118(H11D,H11E,H11F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 204 electrons were 
found in a volume of 2210\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4[C2H5OH] per Formula Unit 
which account for 208 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92732
_shelx_fab_checksum              79188
_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 6.393
_oxdiff_exptl_absorpt_empirical_full_min 0.290