Ordered assembly of two different metal clusters with the same topological connectivity in one single coordination network.
Cao, Jian-Wei; Zhang, Tao; Chen, Juan; Wang, Jin-Bo; Wang, Yu; Chen, Kai-Jie; Chemical science 15 (2024) 11928–11936; doi:10.1039/d4sc02550d

data_1571999
_publ_section_title
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 Ordered assembly of two different metal clusters with the same
 topological connectivity in one single coordination network.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              11928
_journal_page_last               11936
_journal_paper_doi               10.1039/d4sc02550d
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H45 Mn6 N12 O20, 9[C3H7NO]'
_chemical_formula_sum            'C66 H45 Mn6 N12 O20'
_chemical_formula_weight         1655.78
_chemical_name_systematic        NPU-1-TPT
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-21 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1992(13)
_cell_length_b                   29.767(3)
_cell_length_c                   21.8387(18)
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    150.15(10)
_cell_measurement_theta_max      57.075
_cell_measurement_theta_min      2.583
_cell_volume                     11180.7(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15(10)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61016
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.699
_diffrn_reflns_theta_min         2.581
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           2.86
_diffrn_source_power             0.19977099999999998
_diffrn_source_target            Mo
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.971
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1436 before and 0.1008 after correction.
 The Ratio of minimum to maximum transmission is 0.79.

Final HKLF 4 output contains 122079 reflections, Rint = 0.0825
 (49641 with I > 3sig(I), Rint = 0.0704)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11564
_refine_ls_number_restraints     709
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1146P)^2^+96.2289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2085
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                11467
_reflns_number_total             11564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02550d2.cif
_cod_data_source_block           npu-1-tpt
_cod_depositor_comments
'Adding full bibliography for 1571999--1572000.cif.'
_cod_database_code               1571999
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.504(11)
 0.496(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C2-C1 = C8-C5
 1.5 with sigma of 0.01
 C5-C4 = C6-C5 = C7-C6 = C7-C2 = C3-C2 = C4-C3
 1.39 with sigma of 0.01
 O3-C1 = C1-O2 = O5-C8 = C8-O4
 1.25 with sigma of 0.01
 O3-O2 = O5-O4
 2.165 with sigma of 0.02
4. Restrained planarity
 C9, C10, C11, C12, C13, C14, C15, C16
 with sigma of 0.01
 C10A, C11A, C12A, C13A, C14A, C15A, C42, C9A
 with sigma of 0.01
 C2, C3, C7, C5, C4, C6, C1, C8
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
O6 \\sim O7 \\sim O8 \\sim O9 \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim
C13A \\sim C14A \\sim C15A \\sim C42 \\sim O6A \\sim O7A \\sim O8A \\sim O9A
\\sim Mn3 \\sim Mn1: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C18 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C7 \\sim O3 \\sim C8 \\sim C5 \\sim C4 \\sim C6
\\sim O5 \\sim O4 \\sim O2 \\sim Mn1 \\sim Mn2: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O9) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(O6A)
\\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(O9A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C12A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O7A) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
6. Same fragment restrains
{Mn1, Mn3, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C42, O6A, O7A, O8A, O9A}
sigma for 1-2: 0.01, 1-3: 0.02
as in
{Mn1, Mn3, C9, C10, C11, C12, C13, C14, C15, C16, O6, O7, O8, O9}
7. Others
 Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C42)=Sof(O6A)=Sof(O7A)=Sof(O8A)=
 Sof(O9A)=1-FVAR(1)
 Sof(C9)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(O9)=FVAR(1)
 Fixed Sof: C1(0.5) C2(0.5) C7(0.5) H7(0.5) C6(0.5) H6(0.5) C5(0.5) C4(0.5)
 H4(0.5) C3(0.5) H3(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) O2(0.5) O3(0.5)
 C8(0.5) O5(0.5) O4(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3), C24(H24), C25(H25), C21(H21), C22(H22),
 C32(H32), C29(H29), C30(H30), C31(H31), C37(H37), C38(H38), C35(H35), C36(H36),
  C11(H11), C12(H12), C14(H14), C15(H15), C11A(H11A), C12A(H12A), C14A(H14A),
 C15A(H15A)
8.b Fitted hexagon refined as free rotating group:
 C24(C25,N1,C21,C22,C23), C32(C28,C29,C30,N5,C31), C37(C38,C34,C35,C36,N6),
 N4(C26,N2,C27,N3,C33)
8.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1456 electrons were 
found in a volume of 5818\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
9[C3H7NO] per Asymmetric Unit 
which account for 1440 electrons 
per unit cell, which is much more than the experimental 
value of 464 electrons per unit cell for the guest 
[3DMA and 4H2O] per formula unit. 
We attribute this disagreement to the volatile nature 
of the solvent molecules.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85842
_shelx_hkl_checksum              93117
_shelx_fab_checksum              88220
_olex2_submission_special_instructions 'No special instructions were received'