Elucidating the paramagnetic interactions of an inorganic-organic hybrid radical-functionalized Mn-Anderson cluster.
Lin, Chang-Gen; Hutin, Marie; Busche, Christoph; Bell, Nicola L.; Long, De-Liang; Cronin, Leroy; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2350–2353; doi:10.1039/d0dt04149a

data_7706511
_publ_section_title
;
 Elucidating the paramagnetic interactions of an inorganic-organic hybrid
 radical-functionalized Mn-Anderson cluster.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2350
_journal_page_last               2353
_journal_paper_doi               10.1039/d0dt04149a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'3(C16 H36 N +), C18 H26 Al Mo6 O32 3-, 4(C2H3N)'
_chemical_formula_sum            'C74 H146 Al Mo6 N7 O32'
_chemical_formula_weight         2248.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2021-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0446(2)
_cell_length_b                   14.31510(10)
_cell_length_c                   28.3267(2)
_cell_measurement_reflns_used    39841
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.2590
_cell_measurement_theta_min      2.3500
_cell_volume                     9647.33(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.34a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.860
_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    -50.00  25.00   0.50   10.00    --    0.74 -80.00  20.00  150
  2  \w    -23.00  51.00   0.50   10.00    --    0.74  80.00 143.00  148
  3  \w    -26.00  37.00   0.50   10.00    --   -1.99  80.00 143.00  126
  4  \w    -39.00 -14.00   0.50   10.00    --   -1.99 -80.00  20.00   50
  5  \w    -16.00  33.00   0.50   10.00    --    0.74 -99.00 -30.00   98
  6  \w    -17.00  30.00   0.50   10.00    --   -1.99 -99.00 150.00   94
  7  \w    -18.00  30.00   0.50   10.00    --   -1.99 -99.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286298000
_diffrn_orient_matrix_UB_12      0.0064019000
_diffrn_orient_matrix_UB_13      -0.0026788000
_diffrn_orient_matrix_UB_21      0.0006179000
_diffrn_orient_matrix_UB_22      0.0421626000
_diffrn_orient_matrix_UB_23      0.0132267000
_diffrn_orient_matrix_UB_31      0.0082963000
_diffrn_orient_matrix_UB_32      -0.0252431000
_diffrn_orient_matrix_UB_33      0.0214021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            69943
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.937
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.34a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         13155
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+25.7804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11447
_reflns_number_total             13155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04149a2.cif
_cod_data_source_block           cgl0111a
_cod_depositor_comments
'Adding full bibliography for 7706508--7706513.cif.'
_cod_original_cell_volume        9647.34(13)
_cod_database_code               7706511
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AlMo6O30C120N30
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.920
_diffrn_oxdiff_digest_frames
;
0124e3f28ba9aa735601bcc9d85ed0142f00025b90c
;
_diffrn_oxdiff_digest_hkl
;
01da4ffe008ce684d387825388827f8acf93db
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, {H8'A,H8'B} of C8', All O(H) groups
 At 1.2 times of:
  {H17A,H17B} of C17, {H16A,H16B} of C16, {H15A,H15B} of C15, {H13A,H13B} of
  C13, {H12A,H12B} of C12, {H11A,H11B} of C11, {H8A,H8B} of C8, {H7A,H7B} of C7,
   {H5A,H5B} of C5, {H4A,H4B} of C4, {H3A,H3B} of C3, {H2A,H2B} of C2, {H19A,
  H19B} of C19, {H20A,H20B} of C20, {H21A,H21B} of C21, {H23A,H23B} of C23,
  {H24A,H24B} of C24, {H25A,H25B} of C25, {H27A,H27B} of C27, {H28A,H28B} of
  C28, {H29A,H29B} of C29, {H31A,H31B} of C31, {H32A,H32B} of C32, {H33A,H33B}
  of C33
2. Restrained distances
 C7-C8 = C8-C9
 1.5 with sigma of 0.02
 C7-C8' = C8'-C9'
 1.5 with sigma of 0.02
 C9-O15 \\sim C9-O16 \\sim C9'-O15' \\sim C9'-O16'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O15')=Sof(O16')=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(C9')=1-FVAR(1)
 Sof(O15)=Sof(O16)=Sof(H16)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=FVAR(1)
 Fixed Sof: N3(0.85) N4(0.5) N4'(0.2) C22'(0.4) C22(0.6) H22A(0.6) H22B(0.6)
 H22C(0.6) C35(0.7) C35'(0.15) C36(0.7) H36A(0.7) H36B(0.7) H36C(0.7)
 C36'(0.15) C37'(0.2) C38'(0.2) H38D(0.2) H38E(0.2) H38F(0.2) C37(0.5) C38(0.5)
 H38A(0.7) H38B(0.7) H38C(0.7)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C38'(H38D,H38E,H38F), C38(H38A,H38B,H38C)
5.c Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_shelx_res_checksum              11029
_shelx_hkl_checksum              11026
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.912