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_7128102
_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         'C6 H12 K4 Mn Na2 O32.75 W6, 0.25(O)'
_chemical_formula_sum            'C6 H28 K4 Mn Na2 O33 W6'
_chemical_formula_weight         1988.70
_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             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                95.613(3)
_cell_angle_beta                 97.191(3)
_cell_angle_gamma                111.820(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2889(3)
_cell_length_b                   10.7488(3)
_cell_length_c                   18.3923(6)
_cell_measurement_reflns_used    10657
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      30.0060
_cell_measurement_theta_min      3.6740
_cell_volume                     1850.34(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (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      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_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    -62.00  35.00   1.00   25.00    --   12.19 -38.00 -90.00   97
  2  \w    -51.00  40.00   1.00   25.00    --   12.19 -57.00-180.00   91
  3  \w    -11.00  86.00   1.00   25.00    --   12.19  38.00-120.00   97
  4  \w    -17.00  53.00   1.00   25.00    --   12.19 -99.00  60.00   70
  5  \w    -18.00  83.00   1.00   25.00    --   12.19  77.00  90.00  101
  6  \w    -11.00  85.00   1.00   25.00    --   12.19  38.00   0.00   96
  7  \w      7.00  54.00   1.00   25.00    --  -14.07  38.00  90.00   47
  8  \w    -81.00 -33.00   1.00   25.00    --  -14.07 142.00  60.10   48
  9  \w    -90.00 -65.00   1.00   25.00    --  -14.07 154.00-130.49   25
;
_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      -0.0092425000
_diffrn_orient_matrix_UB_12      0.0441097000
_diffrn_orient_matrix_UB_13      -0.0245915000
_diffrn_orient_matrix_UB_21      0.0512035000
_diffrn_orient_matrix_UB_22      -0.0104280000
_diffrn_orient_matrix_UB_23      -0.0195672000
_diffrn_orient_matrix_UB_31      -0.0545978000
_diffrn_orient_matrix_UB_32      -0.0559045000
_diffrn_orient_matrix_UB_33      -0.0236929000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27362
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.479
_exptl_absorpt_correction_T_max  0.0697
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.467
_refine_diff_density_min         -2.415
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         6501
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0332P)^2^+71.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5762
_reflns_number_total             6501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00563d2.cif
_cod_data_source_block           mnw6beta-3
_cod_depositor_comments
'Adding full bibliography for 7128098--7128102.cif.'
_cod_original_cell_volume        1850.35(11)
_cod_database_code               7128102
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Mn W O C K Na'
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.246
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C4-C6B = C4-O25A
 1.54 with sigma of 0.02
 O25B-C5 = O25A-C4
 1.45 with sigma of 0.02
 C4-C6B \\sim C5-C6A
 with sigma of 0.02
 O25B-C5 \\sim O25A-C4
 with sigma of 0.02
 C6B-C4 \\sim C6A-C5
 with sigma of 0.02
3. Rigid bond restraints
 C6B, C4, O25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25B, C5, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C6B \\sim O25A \\sim C4: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O25B \\sim C5 \\sim C6A: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O12W \\sim O10W: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O11W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6W) = Uanis(Na1)
5. Others
 Fixed Sof: Na2(0.5) O10W(0.75) H5BC(0.6) H5BD(0.6) H5AA(0.4) H5AB(0.4)
 H4BC(0.6) H4BD(0.6) H4AA(0.4) H4AB(0.4) O25B(0.6) H25B(0.6) Na3(0.5) Na1(0.75)
 C6B(0.6) H6BA(0.6) H6BB(0.6) H6BC(0.6) C6A(0.4) H6AA(0.4) H6AB(0.4) H6AC(0.4)
 O25A(0.4) H25A(0.4) O7W(0.5) O8W(0.5) O6W(0.25) Na4(0.25) O5W(0.5) O11W(0.25)
 O12W(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5BC,H5BD), C5(H5AA,H5AB), C1(H1A,H1B), C4(H4BC,H4BD),
 C4(H4AA,H4AB)
6.b Idealised Me refined as rotating group:
 C6B(H6BA,H6BB,H6BC), C6A(H6AA,H6AB,H6AC)
6.c Idealised tetrahedral OH refined as rotating group:
 O25B(H25B), O25A(H25A)
;
_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 2.113
_oxdiff_exptl_absorpt_empirical_full_min 0.680