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_7706510
_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
'C34 H58 Mn Mo6 N6 O30, C16 H36 N, C10.9 H24.3 N, C8 H18 N0.6'
_chemical_formula_sum            'C82 H166 Mn Mo6 N9 O30'
_chemical_formula_weight         2388.81
_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                 93.5000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3321(2)
_cell_length_b                   20.0174(4)
_cell_length_c                   34.4565(6)
_cell_measurement_reflns_used    27524
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      25.7450
_cell_measurement_theta_min      2.2740
_cell_volume                     12620.6(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      149.99(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 0.995
_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    -54.00  13.00   0.50    6.00    --   -0.17 -62.00 -26.00  134
  2  \w    -13.00  54.00   0.50    6.00    --   -0.17  62.00 111.00  134
  3  \w    -18.00  28.00   0.50    6.00    --   -0.17 -99.00-180.00   92
  4  \w    -18.00  28.00   0.50    6.00    --   -0.17 -99.00  90.00   92
  5  \w    -48.00  18.00   0.50    6.00    --   -0.17 -77.00 -60.00  132
  6  \w    -61.00  -2.00   0.50    6.00    --   -0.17 -19.00 150.00  118
;
_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      -0.0323190000
_diffrn_orient_matrix_UB_12      0.0188616000
_diffrn_orient_matrix_UB_13      -0.0040201000
_diffrn_orient_matrix_UB_21      0.0172224000
_diffrn_orient_matrix_UB_22      0.0174418000
_diffrn_orient_matrix_UB_23      -0.0148636000
_diffrn_orient_matrix_UB_31      -0.0126759000
_diffrn_orient_matrix_UB_32      -0.0244032000
_diffrn_orient_matrix_UB_33      -0.0137285000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            136630
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.727
_diffrn_reflns_theta_min         2.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             4952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         23990
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.1016
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1156P)^2^+93.5565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.3173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14359
_reflns_number_total             23990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04149a2.cif
_cod_data_source_block           cgl0104_sq
_cod_depositor_comments
'Adding full bibliography for 7706508--7706513.cif.'
_cod_database_code               7706510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo6 Mn N10 C90 O40'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.930
_diffrn_oxdiff_digest_frames
;
0113e6d8e5d9850272fa224b6b614477b40070240ed
;
_diffrn_oxdiff_digest_hkl
;
0189b0a34831ba0f1748d36e012341c84364ea
;
_reflns_odcompleteness_completeness 93.16
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C41 = C41-C42 = C42-C43 = C43-C44
 1.5 with sigma of 0.02
 N7-C45 = C45-C46 = C46-C47 = C47-C48
 1.5 with sigma of 0.02
 N7-C49 = C49-C50 = C50-C51 = C51-C52
 1.5 with sigma of 0.02
 N7-C53 = C53-C54 = C54-C55 = C55-C56
 1.5 with sigma of 0.02
 N8-C57 = C57-C58 = C58-C59 = C59-C60
 1.5 with sigma of 0.02
 N8-C61 = C61-C62 = C62-C63 = C63-C64
 1.5 with sigma of 0.02
 N8-C65 = C65-C66 = C66-C67 = C67-C68
 1.5 with sigma of 0.02
 N8-C69 = C69-C70 = C70-C71 = C71-C72
 1.5 with sigma of 0.02
 N9-C73 = C73-C74 = C74-C75 = C75-C76
 1.5 with sigma of 0.02
 N9-C77 = C77-C78 = C78-C79 = C79-C80
 1.5 with sigma of 0.02
 N9-C81 = C81-C82 = C82-C83 = C83-C84
 1.5 with sigma of 0.02
 N9-C85 = C85-C86 = C86-C87 = C87-C88
 1.5 with sigma of 0.02
 C77-C79 = C82-C84
 2.3 with sigma of 0.02
 C7-C6
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim
C34: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: N9(0.6) C57(0.7) H9AA(0.7) H0BA(0.7) C58(0.7) H1BA(0.7) H2BA(0.7)
 C59(0.7) H3BA(0.7) H4BA(0.7) C60(0.7) H5BA(0.7) H6BA(0.7) H7BA(0.7) C61(0.7)
 H8BA(0.7) H9BA(0.7) C62(0.7) H0CA(0.7) H1CA(0.7) C63(0.7) H2CA(0.7) H3CA(0.7)
 C64(0.7) H4CA(0.7) H5CA(0.7) H6CA(0.7) C65(0.7) H7CA(0.7) H8CA(0.7) C66(0.7)
 H9CA(0.7) H0DA(0.7) C67(0.7) H1DA(0.7) H2DA(0.7) C68(0.7) H3DA(0.7) H4DA(0.7)
 H5DA(0.7) C69(0.7) H6DA(0.7) H7DA(0.7) C70(0.7) H8DA(0.7) H9DA(0.7) C71(0.7)
 H0EA(0.7) H1EA(0.7) C72(0.4) H2EA(0.4) H3EA(0.4) H4EA(0.4) C73(0.5) H5EA(0.5)
 H6EA(0.5) C74(0.5) H7EA(0.5) H8EA(0.5) C75(0.5) H9EA(0.5) H0FA(0.5) C76(0.5)
 H1FA(0.5) H2FA(0.5) H3FA(0.5) C77(0.5) H4FA(0.5) H5FA(0.5) C78(0.5) H6FA(0.5)
 H7FA(0.5) C79(0.5) H8FA(0.5) H9FA(0.5) C80(0.5) H0GA(0.5) H1GA(0.5) H2GA(0.5)
 C81(0.5) H3GA(0.5) H4GA(0.5) C82(0.5) H5GA(0.5) H6GA(0.5) C83(0.5) H7GA(0.5)
 H8GA(0.5) C84(0.5) H9GA(0.5) H0HA(0.5) H1HA(0.5) C85(0.5) H2HA(0.5) H3HA(0.5)
 C86(0.5) H4HA(0.5) H5HA(0.5) C87(0.5) H6HA(0.5) H7HA(0.5) C88(0.5) H8HA(0.5)
 H9HA(0.5) H0IA(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C26(H26)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,
 H10B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C23(H23A,H23B), C24(H24A,H24B), C27(H27A,H27B), C34(H34A,H34B), C41(H,HA),
 C42(HB,HC), C43(HD,HE), C45(HI,HJ), C46(HK,HL), C47(HM,HN), C49(HR,HS), C50(HT,
 HU), C51(HV,HW), C53(H0AA,H1AA), C54(H2AA,H3AA), C55(H4AA,H5AA), C57(H9AA,
 H0BA), C58(H1BA,H2BA), C59(H3BA,H4BA), C61(H8BA,H9BA), C62(H0CA,H1CA),
 C63(H2CA,H3CA), C65(H7CA,H8CA), C66(H9CA,H0DA), C67(H1DA,H2DA), C69(H6DA,H7DA),
  C70(H8DA,H9DA), C71(H0EA,H1EA), C73(H5EA,H6EA), C74(H7EA,H8EA), C75(H9EA,
 H0FA), C77(H4FA,H5FA), C78(H6FA,H7FA), C79(H8FA,H9FA), C81(H3GA,H4GA),
 C82(H5GA,H6GA), C83(H7GA,H8GA), C85(H2HA,H3HA), C86(H4HA,H5HA), C87(H6HA,H7HA)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N5(H5)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C44(HF,HG,HH), C48(HO,HP,HQ), C52(HX,HY,HZ), C56(H6AA,H7AA,H8AA),
 C60(H5BA,H6BA,H7BA), C64(H4CA,H5CA,H6CA), C68(H3DA,H4DA,H5DA), C72(H2EA,H3EA,
 H4EA), C76(H1FA,H2FA,H3FA), C80(H0GA,H1GA,H2GA), C84(H9GA,H0HA,H1HA), C88(H8HA,
 H9HA,H0IA)
;
_shelx_res_checksum              74845
_shelx_hkl_checksum              54395
_shelx_fab_checksum              23520
_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 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.813