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_7706512
_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
'C36 H60 Al Mo6 N4 O32, 0.5(C3 H8 N O), C16 H36 N, C16 H27 N'
_chemical_formula_sum            'C87 H175 Al Mo6 N8 O33'
_chemical_formula_weight         2463.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 105.212(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.7469(11)
_cell_length_b                   12.8751(4)
_cell_length_c                   28.9950(7)
_cell_measurement_reflns_used    13550
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.9210
_cell_measurement_theta_min      2.4220
_cell_volume                     12156.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_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      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -10.00  62.00   0.50   10.00    --   -0.17  47.00-130.00  144
  2  \w    -62.00  10.00   0.50   10.00    --   -0.17 -47.00  80.00  144
  3  \w    -18.00  32.00   0.50   10.00    --   -0.17 -99.00  30.00  100
  4  \w    -18.00  32.00   0.50   10.00    --   -0.17 -99.00-180.00  100
  5  \w    -64.00 -20.00   0.50   10.00    --   -0.17 -37.00-180.00   88
  6  \w    -64.00  15.00   0.50   10.00    --   -0.17 -37.00 -90.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0125038000
_diffrn_orient_matrix_UB_12      -0.0286136000
_diffrn_orient_matrix_UB_13      0.0116696000
_diffrn_orient_matrix_UB_21      -0.0176661000
_diffrn_orient_matrix_UB_22      0.0141265000
_diffrn_orient_matrix_UB_23      -0.0182620000
_diffrn_orient_matrix_UB_31      0.0024267000
_diffrn_orient_matrix_UB_32      -0.0449005000
_diffrn_orient_matrix_UB_33      -0.0131604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            135863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
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    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             5128
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.044
_refine_diff_density_max         6.744
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         23867
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0899
_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^)+(0.1050P)^2^+124.6089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16452
_reflns_number_total             23867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04149a2.cif
_cod_data_source_block           cgl0113_sq
_cod_depositor_comments
'Adding full bibliography for 7706508--7706513.cif.'
_cod_database_code               7706512
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AlMo6O35C60N10
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.855
_diffrn_oxdiff_digest_frames
;
0161ea4d0ccaa97dae6fec9f47af657d8000734e520
;
_diffrn_oxdiff_digest_hkl
;
014ee52a0abb64c397cb795e52d37515563ea1
;
_reflns_odcompleteness_completeness 96.34
_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, All O(H) groups
2. Restrained distances
 N5-C49
 1.5 with sigma of 0.02
 C33-C34 = C66-C67 = C67-C68 = C66-C67' = C67'-C68' = C71-C72
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O28) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq,
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Sof(C67')=Sof(C68')=1-FVAR(1)
 Sof(C67)=Sof(C68)=FVAR(1)
 Fixed Sof: O33(0.5) H33(0.5) N7(0.5) C73(0.5) H73(0.5) C74(0.5) H74A(0.5)
 H74B(0.5) H74C(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C28(H28)
5.b 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), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B), C36(H36A,
 H36B), 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),
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C73(H73)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C),
 C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C72(H72A,H72B,
 H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C)
5.e Idealised tetrahedral OH refined as rotating group:
 O33(H33)
;
_shelx_res_checksum              57240
_shelx_hkl_checksum              22820
_shelx_fab_checksum              35767
_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 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.762