Bulky ligands shape the separation between the large spin carriers to condition field-induced slow magnetic relaxation.
Kobylarczyk, Jedrzej; Liberka, Michal; Konieczny, Piotr; Baran, Stanisław; Kubicki, Maciej; Korzeniak, Tomasz; Podgajny, Robert; Dalton transactions (Cambridge, England : 2003) 49 (2020) 300–311; doi:10.1039/c9dt03903a

data_7701981
_publ_section_title
;
 Bulky ligands shape the separation between the large spin carriers to
 condition field-induced slow magnetic relaxation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              300
_journal_page_last               311
_journal_paper_doi               10.1039/c9dt03903a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C198 H220 Mn9 N64 O8 W6, 4(C6 H14 O), 2(H2 O)'
_chemical_formula_sum            'C222 H280 Mn9 N64 O14 W6'
_chemical_formula_weight         5666.64
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-17 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                82.386(5)
_cell_angle_beta                 74.694(5)
_cell_angle_gamma                86.907(4)
_cell_formula_units_Z            1
_cell_length_a                   16.0808(10)
_cell_length_b                   20.4138(10)
_cell_length_c                   20.5125(13)
_cell_measurement_reflns_used    10359
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.1560
_cell_measurement_theta_min      3.4460
_cell_volume                     6436.3(7)
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_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    'SIR97 (Burla et al.,  2007)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.1395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112115
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.021
_exptl_absorpt_coefficient_mu    3.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2841
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.520
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1455
_refine_ls_number_reflns         22598
_refine_ls_number_restraints     820
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0189P)^2^+27.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14381
_reflns_number_total             22598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03903a2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7701980--7701982.cif.'
_cod_database_code               7701981
_shelx_shelxl_version_number     2017/1
_audit_contact_author
;
Maciej Kubicki   
Faculty of Chemistry 
Adam Mickiewicz University
Grunwaldzka 6              
60-780 Pozna\'n   
Poland             
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2SA,H2SB,H2SC} of C2S, {H3SA,H3SB,H3SC} of C3S, {H5SA,
  H5SB,H5SC} of C5S, {H6SA,H6SB,H6SC} of C6S, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  {H85A,H85B,H85C} of C85, {H86A,H86B,H86C} of C86, {H10D,H10E,H10F} of C104,
  {H10G,H10H,H10I} of C105, {H95A,H95B,H95C} of C95, {H93A,H93B,H93C} of C93,
  {H94A,H94B,H94C} of C94, {H11G,H11H,H11I} of C113, {H10A,H10B,H10C} of C106,
  {H11A,H11B,H11C} of C115, {H11D,H11E,H11F} of C114, {H8SA,H8SB,H8SC} of C8S,
  {H9SA,H9SB,H9SC} of C9S, {H11J,H11K,H11L} of C11S, {H12A,H12B,H12C} of C12S,
  {H54A,H54B,H54C} of C54, {H55A,H55B,H55C} of C55, {H45A,H45B,H45C} of C45,
  {H65A,H65B,H65C} of C65, {H53A,H53B,H53C} of C53, {H46A,H46B,H46C} of C46,
  {H66A,H66B,H66C} of C66, {H64A,H64B,H64C} of C64, {H44A,H44B,H44C} of C44,
  {H73A,H73B,H73C} of C73, {H75A,H75B,H75C} of C75, {H74A,H74B,H74C} of C74,
  {H84A,H84B,H84C} of C84, {H2A,H2B,H2C} of C2, {H3A,H3B,H3C} of C3, {H4A,H4B,
  H4C} of C4
2. Restrained distances
 C83-C86 = C72-C75 = C72-C73
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O3S) \\sim Ueq, Uanis(C7S)
\\sim Ueq, Uanis(C8S) \\sim Ueq, Uanis(C9S) \\sim Ueq, Uanis(C10S) \\sim Ueq,
Uanis(C11S) \\sim Ueq, Uanis(C12S) \\sim Ueq, Uanis(N36) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(N23) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C75) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.01
Uanis(C86) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 N40, N41, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, C51, C52,
 C53, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N100, N101, C100, C101, C102, C103, C104, C105, C106, C107, C108, C109, C110,
 C111, C112, C113, C114, C115, C116, C117
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O3S, C7S, C8S, C9S, C10S, C11S, C12S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N60, N61, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69, C70, C71, C72,
 C73, C74, C75, C76, C77
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N80, N81, C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92,
 C93, C94, C95, C96, C97
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{O3S, C7S, C9S, C8S, C10S, C11S, C12S} sigma for 1-2: 0.01, 1-3: 0.01
as
{O2S, C1S, C2S, C3S, C4S, C5S, C6S}
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2), O3(H3), O4(H4), O1S(H1SA,H1SB)
6.b Ternary CH refined with riding coordinates:
 C1S(H1S), C4S(H4S), C7S(H7S), C10S(H10S)
6.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C41(H41), C47(H47), C50(H50), C56(H56), C57(H57), C60(H60),
 C61(H61), C67(H67), C70(H70), C76(H76), C77(H77), C80(H80), C81(H81), C87(H87),
  C90(H90), C96(H96), C97(H97), C100(H100), C101(H101), C107(H107), C110(H110),
 C116(H116), C117(H117)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C93(H93A,H93B,
 H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C104(H10D,H10E,H10F),
 C105(H10G,H10H,H10I), C106(H10A,H10B,H10C), C113(H11G,H11H,H11I), C114(H11D,
 H11E,H11F), C115(H11A,H11B,H11C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC),
 C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,H8SC), C9S(H9SA,H9SB,
 H9SC), C11S(H11J,H11K,H11L), C12S(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'