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_7706513
_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 +), C10 H18 Al Mo6 O26 3-, C3 H7 N O'
_chemical_formula_sum            'C61 H133 Al Mo6 N4 O27'
_chemical_formula_weight         1957.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-04
_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                 90.0190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4262(2)
_cell_length_b                   54.1958(7)
_cell_length_c                   23.3363(3)
_cell_measurement_reflns_used    51243
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.9010
_cell_measurement_theta_min      2.2940
_cell_volume                     19510.0(4)
_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 0.999
_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    -18.00  36.00   0.40    5.00    --   -1.81 -99.00  90.00  135
  2  \w    -65.00  17.00   0.40    5.00    --   -1.81 -57.00 -60.00  205
  3  \w    -64.00  20.00   0.40    5.00    --   -0.69 -57.00   0.00  210
  4  \w    -18.00  38.00   0.40    5.00    --   -0.69 -99.00 150.00  140
  5  \w    -69.00 -43.80   0.40    5.00    --   -0.69 -37.00-120.00   63
  6  \w    -65.00  17.00   0.40    5.00    --   -1.81 -57.00-150.00  205
;
_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      -0.0454905000
_diffrn_orient_matrix_UB_12      0.0007675000
_diffrn_orient_matrix_UB_13      0.0041063000
_diffrn_orient_matrix_UB_21      -0.0064857000
_diffrn_orient_matrix_UB_22      -0.0013952000
_diffrn_orient_matrix_UB_23      -0.0299209000
_diffrn_orient_matrix_UB_31      -0.0020051000
_diffrn_orient_matrix_UB_32      -0.0129857000
_diffrn_orient_matrix_UB_33      0.0034385000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            225200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.705
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.34a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             8064
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1409
_refine_ls_number_reflns         37058
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+172.7064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25372
_reflns_number_total             37058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04149a2.cif
_cod_data_source_block           cgl0111_sq
_cod_depositor_comments
'Adding full bibliography for 7706508--7706513.cif.'
_cod_database_code               7706513
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo6 Al O30 N10 C90 H200'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.923
_diffrn_oxdiff_digest_frames
;
018e1fef1db804fa6ef01797cdbb3f13ea0095899e0
;
_diffrn_oxdiff_digest_hkl
;
01a3f3dc4972c7a051d27fc89dea76d71e5cfe
;
_reflns_odcompleteness_completeness 92.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C10-O26 = C10-O26'
 1.4 with sigma of 0.02
 C23-C24
 1.5 with sigma of 0.02
 C46-C47 = C47-C48
 1.5 with sigma of 0.02
 N3-C61 = C61-C62 = C62-C63 = C63-C64
 1.5 with sigma of 0.02
 C66-C67
 1.5 with sigma of 0.02
 C73-C74
 1.5 with sigma of 0.02
 C78-C79 = C79-C80 = C82-C83 = C83-C84
 1.5 with sigma of 0.02
 N5-C85 = C85-C86 = C86-C87 = C87-C88
 1.5 with sigma of 0.02
 N5-C89 = C89-C90 = C90-C91 = C91-C92
 1.5 with sigma of 0.02
 N5-C93 = C93-C94 = C94-C95 = C95-C96
 1.5 with sigma of 0.02
 N5-C97 = C97-C98 = C98-C99 = C99-C100
 1.5 with sigma of 0.02
 N6-C102 = N6-C103
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: O26(0.5) H26(0.5) O26'(0.5) H26'(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
 C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C51(0.5)
 H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C55(0.5) H55A(0.5)
 H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C64(0.5) H64A(0.5) H64B(0.5)
 H64C(0.5) C67(0.5) H67(0.5) C68(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C72(0.5)
 H72A(0.5) H72B(0.5) H72C(0.5) C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5)
 H75B(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) C80(0.5) H80A(0.5) H80B(0.5)
 H80C(0.5) C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5)
 C85(0.5) H85A(0.5) H85B(0.5) C86(0.5) H86A(0.5) H86B(0.5) C87(0.5) H87A(0.5)
 H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5) H88C(0.5) C92(0.5) H92A(0.5) H92B(0.5)
 H92C(0.5) C94(0.5) H94A(0.5) H94B(0.5) C95(0.5) H95A(0.5) H95B(0.5) C96(0.5)
 H96A(0.5) H96B(0.5) H96C(0.5) C98(0.5) H98A(0.5) H98B(0.5) C99(0.5) H99A(0.5)
 H99B(0.5) C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C102(0.5) H10D(0.5)
 H10E(0.5) H10F(0.5)
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B),
  C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,
 H65B), C66(H66A,H66B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B), C78(H78A,H78B),
  C79(H79A,H79B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C89(H89A,H89B), C90(H90A,H90B),
 C91(H91A,H91B), C94(H94A,H94B), C95(H95A,H95B), C98(H98A,H98B), C99(H99A,H99B)
4.c Aromatic/amide H refined with riding coordinates:
 C67(H67), C101(H101)
4.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C36(H36A,H36B,
 H36C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C52(H52A,
 H52B,H52C), C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C),
 C68(H68A,H68B,H68C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C80(H80A,H80B,
 H80C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C), C92(H92A,H92B,H92C), C96(H96A,
 H96B,H96C), C100(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,H10H,H10I)
4.e Idealised tetrahedral OH refined as rotating group:
 O13(H13), O26(H26), O26'(H26'), O51(H51), O52(H52)
;
_shelx_res_checksum              68334
_shelx_hkl_checksum              53163
_shelx_fab_checksum              79260
_platon_squeeze_void_probe_radius 1.20
_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 1.059
_oxdiff_exptl_absorpt_empirical_full_min 0.936