Unprecedented monofunctionalized β-Anderson clusters: [R<sub>1</sub>R<sub>2</sub>C(CH<sub>2</sub>O)<sub>2</sub>Mn<sup>IV</sup>W<sub>6</sub>O<sub>22</sub>]<sup>6-</sup>, a class of potential candidates for new inorganic linkers.
Li, Qi; Wei, Yongge; Chemical communications (Cambridge, England) 57 (2021) 3865–3868; doi:10.1039/d1cc00563d

data_7128099
_publ_section_title
;
 Unprecedented monofunctionalized \b-Anderson clusters:
 [R<sub>1</sub>R<sub>2</sub>C(CH<sub>2</sub>O)<sub>2</sub>Mn<sup>IV</sup>W<sub>6</sub>O<sub>22</sub>]<sup>6-</sup>,
 a class of potential candidates for new inorganic linkers.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3865
_journal_page_last               3868
_journal_paper_doi               10.1039/d1cc00563d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C4 H10 K3.5 Mn N Na1.5 O32 W6, 2.75(O)'
_chemical_formula_sum            'C4 H29.5 K3.5 Mn N Na1.5 O34.75 W6'
_chemical_formula_weight         1977.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-01 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.226(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8017(9)
_cell_length_b                   12.0565(7)
_cell_length_c                   17.3015(10)
_cell_measurement_reflns_used    4606
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0890
_cell_measurement_theta_min      3.9610
_cell_volume                     3468.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -20.00  52.00   1.00    8.00    --   12.19 -99.00-120.00   72
  2  \w    -71.00 -17.00   1.00    8.00    --  -14.07 -38.00  90.00   54
  3  \w    -87.00   6.00   1.00    8.00    --  -14.07 -57.00  30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0130031000
_diffrn_orient_matrix_UB_12      0.0314760000
_diffrn_orient_matrix_UB_13      0.0341222000
_diffrn_orient_matrix_UB_21      0.0139902000
_diffrn_orient_matrix_UB_22      -0.0491852000
_diffrn_orient_matrix_UB_23      0.0200280000
_diffrn_orient_matrix_UB_31      0.0381248000
_diffrn_orient_matrix_UB_32      0.0073365000
_diffrn_orient_matrix_UB_33      -0.0122856000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16183
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.333
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.720
_exptl_absorpt_correction_T_max  0.0696
_exptl_absorpt_correction_T_min  0.0415
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    3.786
_exptl_crystal_description       plate
_exptl_crystal_F_000             3562
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6105
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0333P)^2^+12.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4867
_reflns_number_total             6105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00563d2.cif
_cod_data_source_block           mnw6beta-2
_cod_depositor_comments
'Adding full bibliography for 7128098--7128102.cif.'
_cod_original_formula_sum        'C4 H29.50 K3.50 Mn N Na1.50 O34.75 W6'
_cod_database_code               7128099
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Mn W O C N K Na'
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.231
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3WB) \\sim Ueq, Uanis(O3WA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O6WB) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6WA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O6WA(0.5) Na1(0.5) O3WB(0.5) O6WB(0.25) O1W(0.5) O3WA(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C4(H4A,H4B)
4.b Idealised Me refined as rotating group:
 N35(H35A,H35B,H35C)
4.c Idealised tetrahedral OH refined as rotating group:
 O25(H25)
;
_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 3.305
_oxdiff_exptl_absorpt_empirical_full_min 0.511