From cubane-assembled Mn-oxo clusters to monodispersed manganese oxide colloidal nanocrystals.
He, Yan; Liu, Yang; Zheng, Huijuan; Xiang, Zhen; Zhou, Zheng; Geng, Fengting; Geng, Longlong; Dikarev, Evgeny V.; Han, Haixiang; Chemical science 15 (2024) 10381–10391; doi:10.1039/d4sc01451k

data_1571814
_publ_section_title
;
 From cubane-assembled Mn-oxo clusters to monodispersed manganese oxide
 colloidal nanocrystals.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              10381
_journal_page_last               10391
_journal_paper_doi               10.1039/d4sc01451k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C48 H88 Mn18 N2 O48'
_chemical_formula_sum            'C50 H96 Mn18 N2 O50'
_chemical_formula_weight         2514.20
_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             2024-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-01-12 deposited with the CCDC.	2024-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.181(3)
_cell_angle_beta                 99.194(4)
_cell_angle_gamma                90.133(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4312(5)
_cell_length_b                   13.1605(6)
_cell_length_c                   16.2948(8)
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    160
_cell_measurement_theta_max      70.532
_cell_measurement_theta_min      2.864
_cell_volume                     2118.14(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32244
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.628
_diffrn_reflns_theta_min         2.864
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    21.854
_exptl_absorpt_correction_T_max  0.3241
_exptl_absorpt_correction_T_min  0.2029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1472 before and 0.0959 after correction.
The Ratio of minimum to maximum transmission is 0.6260.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8321
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4404
_reflns_number_total             8321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01451k2.cif
_cod_data_source_block           hh_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1571813--1571814.cif.'
_cod_database_code               1571814
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N1, C41, C46, C43, C38, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C48 \\sim O48 \\sim C22 \\sim O45 \\sim Mn18: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C48 \\sim C22 \\sim O45 \\sim O48: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C30 \\sim C38 \\sim C43 \\sim C46 \\sim C41 \\sim N1 \\sim Mn16: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C48) = Uanis(C22) = Uanis(O48) = Uanis(O45)
Uanis(O48) = Uanis(C22) = Uanis(O45)
4. Rigid body (RIGU) restrains
 Mn15, Mn18, O3, O31, O22, O42, O45, C27, C10, C15, C22, C26, C39, O48, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C41(H41), C38(H38), C43(H43), C46(H46)
5.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C10(H10a,H10b,H10c), C29(H29a,H29b,H29c), C15(H15a,H15b,
 H15c), C31(H31a,H31b,H31c), C18(H18a,H18b,H18c), C33(H33a,H33b,H33c), C35(H35a,
 H35b,H35c), C39(H39a,H39b,H39c), C34(H34a,H34b,H34c), C42(H42a,H42b,H42c),
 C45(H45a,H45b,H45c), C48(H48a,H48b,H48c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 40 electrons were 
found in a volume of 188\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH3OH] per Asymmetric Unit 
which account for 36 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              827
_shelx_hkl_checksum              31249
_shelx_fab_checksum              52964
_olex2_submission_special_instructions 'No special instructions were received'