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_1572000
_publ_section_title
;
 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_formula_moiety         'C108 H69 Mn9 N18 O33'
_chemical_formula_sum            'C108 H69 Mn9 N18 O33'
_chemical_formula_weight         2641.27
_chemical_name_systematic        NPU-6
_space_group_crystal_system      hexagonal
_space_group_IT_number           187
_space_group_name_Hall           'P -6 2'
_space_group_name_H-M_alt        'P -6 m 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-06-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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                120
_cell_formula_units_Z            1
_cell_length_a                   17.1984(7)
_cell_length_b                   17.1984(7)
_cell_length_c                   18.6767(10)
_cell_measurement_reflns_used    7471
_cell_measurement_temperature    198.15(10)
_cell_measurement_theta_max      25.875
_cell_measurement_theta_min      2.369
_cell_volume                     4784.2(4)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      198.15(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63019
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.181
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.0289
_exptl_absorpt_correction_T_min  0.0101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0991 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.3495.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.917
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 1558 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3615
_reflns_number_total             4160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02550d2.cif
_cod_data_source_block           npu-6
_cod_depositor_comments
'Adding full bibliography for 1571999--1572000.cif.'
_cod_original_cell_volume        4784.2(5)
_cod_database_code               1572000
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52364
 0.47636
2. Uiso/Uaniso restraints and constraints
C7 \\sim C10 \\sim C8 \\sim C9 \\sim C8A \\sim C9A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
3. Same fragment restrains
{C7, C10, C8A, C9A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C7, C10, C8, C9}
4. Others
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=FVAR(1)
 Fixed Sof: H13A(0.25) H13B(0.25) H13C(0.25)
5.a Riding coordinates:
 C13(H13A,H13B,H13C), C15(H15)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C8(H8), C9(H9), C14(H14), C8A(H8A), C9A(H9A)
;
_smtbx_masks_special_details
;

A solvent mask was calculated and 695 electrons 
were found in a volume of 2548\%A^3^ in 1 void 
per unit cell, which is much more than the experimental 
value of of 1[12'C4H9NO'9'H2O] per unit cell
which account for 122 electrons per unit cell. 
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              72183
_shelx_hkl_checksum              34639
_shelx_fab_checksum              74953
_olex2_submission_special_instructions 'No special instructions were received'