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_7706508
_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
'2(C18 H31 Mn0.5 Mo3 N3 O15), 4(C3 H7 N O), 3(C16 H36 N)'
_chemical_formula_sum            'C96 H198 Mn Mo6 N13 O34'
_chemical_formula_weight         2709.24
_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             2020-05-04
_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                71.6880(10)
_cell_angle_beta                 79.9100(10)
_cell_angle_gamma                74.2640(10)
_cell_formula_units_Z            2
_cell_length_a                   18.48700(10)
_cell_length_b                   19.4071(2)
_cell_length_c                   19.6357(2)
_cell_measurement_reflns_used    70041
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.4020
_cell_measurement_theta_min      2.2490
_cell_volume                     6406.17(11)
_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)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.905
_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    -15.00  57.80   0.65    3.00    --   -0.17  57.00-120.00  112
  2  \w    -23.00   2.35   0.65    3.00    --   -0.17  77.00 -60.00   39
  3  \w    -25.00  64.05   0.65    3.00    --   -0.17  19.00-150.00  137
  4  \w    -15.00  63.00   0.65    3.00    --   -0.17  37.00 -30.00  120
  5  \w    -23.00  49.80   0.65    3.00    --   -0.17  77.00  30.00  112
  6  \w    -15.00  57.80   0.65    3.00    --   -0.17  57.00  90.00  112
  7  \w    -21.00  51.80   0.65    3.00    --   -0.17  73.00 158.00  112
  8  \w    -59.00  14.45   0.65    3.00    --   -0.17 -57.00 -90.00  113
  9  \w    -53.00  19.80   0.65    3.00    --   -0.17 -73.00  29.00  112
 10  \w    -18.00  31.40   0.65    3.00    --   -0.17 -99.00 150.00   76
;
_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      0.0078241000
_diffrn_orient_matrix_UB_12      0.0330237000
_diffrn_orient_matrix_UB_13      0.0021720000
_diffrn_orient_matrix_UB_21      -0.0194913000
_diffrn_orient_matrix_UB_22      0.0208355000
_diffrn_orient_matrix_UB_23      -0.0308162000
_diffrn_orient_matrix_UB_31      -0.0341082000
_diffrn_orient_matrix_UB_32      0.0064165000
_diffrn_orient_matrix_UB_33      0.0225301000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            169448
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.462
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87368
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1332
_refine_ls_number_reflns         35252
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0450P)^2^+6.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28074
_reflns_number_total             35252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04149a2.cif
_cod_data_source_block           cgl0105_2_sq
_cod_depositor_comments
'Adding full bibliography for 7706508--7706513.cif.'
_cod_original_cell_volume        6406.18(11)
_cod_database_code               7706508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo Mn6 O40'
_chemical_oxdiff_usercomment     'flat plate'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.930
_diffrn_oxdiff_digest_frames
;
019ca561b523391af98be328bfacc6d881000268e72
;
_diffrn_oxdiff_digest_hkl
;
01e64887ee8734721dce167546b3ea2d04628e
;
_reflns_odcompleteness_completeness 99.92
_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
 C68-C67 = C60-C59 = C80-C79 = C84-C83 = C72-C71
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
4.a Ternary CH refined with riding coordinates:
 C10(H10), C28(H28)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C11(H11A,H11B), C15(H15A,H15B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B),
  C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B), C30(H30A,
 H30B), 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),
  C67(H67A,H67B), 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)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N5(H5), C85(H85), C88(H88), C91(H91), C94(H94)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), 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), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C),
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C93(H93A,H93B,
 H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              84248
_shelx_hkl_checksum              19706
_shelx_fab_checksum              4255
_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 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.708