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_7701982
_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         '2(C124 H80 Mn4.5 N32 O4 W3), 6(O), 29(C O)'
_chemical_formula_sum            'C277 H159 Mn9 N64 O43 W6'
_chemical_formula_weight         6669.23
_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     dual
_audit_creation_date             2019-05-11
_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                89.0040(10)
_cell_angle_beta                 83.0100(10)
_cell_angle_gamma                87.2110(10)
_cell_formula_units_Z            2
_cell_length_a                   24.8236(9)
_cell_length_b                   25.1491(8)
_cell_length_c                   25.8948(9)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    117(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.53
_cell_volume                     16025.7(10)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      117
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            201199
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.254
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0852 before and 0.0620 after correction. The Ratio of minimum to maximum transmission is 0.8041. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             6564
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.069
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3475
_refine_ls_number_reflns         56317
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+131.7751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                39502
_reflns_number_total             56317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03903a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7701980--7701982.cif.'
_cod_database_code               7701982
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O31S-C31S
 1.4 with sigma of 0.02
 C32S-O32S
 1.4 with sigma of 0.02
 C39S-O39S
 1.4 with sigma of 0.02
 C52S-O52S
 1.4 with sigma of 0.02
 O15S-C15S
 1.4 with sigma of 0.02
 C33S-O33S
 1.4 with sigma of 0.02
 C43S-O43S
 1.4 with sigma of 0.02
 C20S-O20S
 1.4 with sigma of 0.02
 O3M-H3M
 0.87 with sigma of 0.01
 O1M-H1M
 0.87 with sigma of 0.01
 O4M-H4M
 0.87 with sigma of 0.01
 O8M-H8M
 0.87 with sigma of 0.01
 O5M-H5M
 0.87 with sigma of 0.01
 O6M-H6M
 0.87 with sigma of 0.01
 C2N-O2M
 1.4 with sigma of 0.02
 O2M-H2MA
 0.87 with sigma of 0.01
 O2M-H2M
 0.87 with sigma of 0.01
 H2M-O45S
 -2.5 with sigma of 0.02
 C7M-O7M
 1.4 with sigma of 0.02
 O10S-C10S = O11S-C11S
 1.4 with sigma of 0.02
 C9S-O9S
 1.4 with sigma of 0.02
 O24S-C24S
 1.4 with sigma of 0.02
 C36S-O36S
 1.4 with sigma of 0.02
 O38S-C38S
 1.4 with sigma of 0.02
 C40S-O40S
 1.4 with sigma of 0.02
 O49S-C49S
 1.4 with sigma of 0.02
 C26S-O26S
 1.4 with sigma of 0.02
 O50S-C50S
 1.4 with sigma of 0.02
 O35S-C35S
 1.4 with sigma of 0.02
 O34S-C34S
 1.4 with sigma of 0.02
 O42S-C42S
 1.4 with sigma of 0.02
 C23S-O23S
 1.4 with sigma of 0.02
 O46S-C46S
 1.4 with sigma of 0.02
 O21S-C21S
 1.4 with sigma of 0.02
 C22S-O22S
 1.4 with sigma of 0.02
 O53S-C53S
 1.4 with sigma of 0.02
 O36S-C36S
 1.4 with sigma of 0.02
 O33S-C33S
 1.4 with sigma of 0.02
 O51S-C51S
 1.4 with sigma of 0.02
 C29S-O29S
 1.4 with sigma of 0.02
 O16S-C16S
 1.4 with sigma of 0.02
 O23S-C23S
 1.4 with sigma of 0.02
 C24S-O24S
 1.4 with sigma of 0.02
 O8SB-C8S
 1.4 with sigma of 0.02
 C12S-O12S
 1.4 with sigma of 0.02
 O14S-C14S
 1.4 with sigma of 0.02
 O53S-N16A
 -2.8 with sigma of 0.02
 N16A-O53S
 -2.7 with sigma of 0.02
 H507-H2MA_$1
 -2.5 with sigma of 0.02
 O25S-C0AA
 1.4 with sigma of 0.02
 C3M-H3M
 1.917319 with sigma of 0.02
 Mn4A-H3M
 2.826625 with sigma of 0.02
 C1M-H1M
 1.937186 with sigma of 0.02
 Mn2A-H1M
 2.784237 with sigma of 0.02
 C4M-H4M
 1.925893 with sigma of 0.02
 Mn5A-H4M
 2.895203 with sigma of 0.02
 C8M-H8M
 1.908449 with sigma of 0.02
 Mn5B-H8M
 2.825686 with sigma of 0.02
 C5M-H5M
 1.923001 with sigma of 0.02
 Mn2B-H5M
 2.936296 with sigma of 0.02
 C6M-H6M
 1.906655 with sigma of 0.02
 Mn3B-H6M
 2.801448 with sigma of 0.02
 C2M-H2MA
 1.865423 with sigma of 0.02
 Mn3A-H2MA
 2.856665 with sigma of 0.02
 C2N-H2M
 1.911903 with sigma of 0.02
 Mn3A-H2M
 2.786143 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N31A \\sim C31A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
N15B \\sim C15B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O2M \\sim C2N: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
O7M \\sim C7M: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C31A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.2
Uanis(C15B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.2
Uanis(C11A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.2
Uanis(C2N) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C33B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: H2M(0.5) H2MA(0.5) O2S(0.5) O5S(0.5) O6S(0.5) O7S(0.5) O8SA(0.75)
 O8SB(0.25) O9S(0.5) O10S(0.25) O11S(0.25) O15S(0.5) O16S(0.75) O19S(0.5)
 O20S(0.25) O21S(0.25) O22S(0.5) C0AA(0.25) O26S(0.5) O27S(0.5) O31S(0.5)
 O32S(0.5) O33S(0.5) O34S(0.5) O35S(0.5) O36S(0.5) O38S(0.25) O39S(0.25)
 O40S(0.25) O43S(0.5) O44S(0.25) O45S(0.5) O46S(0.5) O49S(0.25) O50S(0.5)
 O52S(0.5) O53S(0.25) C2M(0.5) H2MB(0.5) H2MC(0.5) H2MD(0.5) C2N(0.5) H2NA(0.5)
 H2NB(0.5) H2NC(0.5) C7M(0.4) H7MA(0.4) H7MB(0.4) H7MC(0.4) C7N(0.6) H7NA(0.6)
 H7NB(0.6) H7NC(0.6) C9S(0.5) C10S(0.25) C11S(0.25) C15S(0.5) C16S(0.75)
 C19S(0.5) C20S(0.25) C21S(0.25) C22S(0.5) O25S(0.25) C26S(0.5) C27S(0.5)
 C31S(0.5) C32S(0.5) C33S(0.5) C34S(0.5) C35S(0.5) C36S(0.5) C38S(0.25)
 C39S(0.25) C40S(0.25) C43S(0.5) C44S(0.25) C45S(0.5) C46S(0.5) C49S(0.25)
 C50S(0.5) C52S(0.5) C53S(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C100(H100), C101(H101), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108), C110(H110), C111(H111), C115(H115), C116(H116), C117(H117),
 C118(H118), C119(H119), C120(H120), C121(H121), C200(H200), C201(H201),
 C204(H204), C205(H205), C206(H206), C207(H207), C208(H208), C210(H210),
 C211(H211), C215(H215), C216(H216), C217(H217), C218(H218), C219(H219),
 C220(H220), C221(H221), C300(H300), C301(H301), C304(H304), C305(H305),
 C306(H306), C307(H307), C308(H308), C310(H310), C311(H311), C315(H315),
 C316(H316), C317(H317), C318(H318), C319(H319), C320(H320), C321(H321),
 C400(H400), C401(H401), C404(H404), C405(H405), C406(H406), C407(H407),
 C408(H408), C410(H410), C411(H411), C415(H415), C416(H416), C417(H417),
 C418(H418), C419(H419), C420(H420), C421(H421), C500(H500), C501(H501),
 C504(H504), C505(H505), C506(H506), C507(H507), C508(H508), C510(H510),
 C511(H511), C515(H515), C516(H516), C517(H517), C518(H518), C519(H519),
 C520(H520), C521(H521), C600(H600), C601(H601), C604(H604), C605(H605),
 C606(H606), C607(H607), C608(H608), C610(H610), C611(H611), C615(H615),
 C616(H616), C617(H617), C618(H618), C619(H619), C620(H620), C621(H621),
 C700(H700), C701(H701), C704(H704), C705(H705), C706(H706), C707(H707),
 C708(H708), C710(H710), C711(H711), C715(H715), C716(H716), C717(H717),
 C718(H718), C719(H719), C720(H720), C721(H721), C800(H800), C801(H801),
 C804(H804), C805(H805), C806(H806), C807(H807), C808(H808), C810(H810),
 C811(H811), C815(H815), C816(H816), C817(H817), C818(H818), C819(H819),
 C820(H820), C821(H821)
5.b Idealised Me refined as rotating group:
 C1M(H1MA,H1MB,H1MC), C2M(H2MB,H2MC,H2MD), C2N(H2NA,H2NB,H2NC), C3M(H3MA,H3MB,
 H3MC), C4M(H4MA,H4MB,H4MC), C5M(H5MA,H5MB,H5MC), C6M(H6MA,H6MB,H6MC), C7M(H7MA,
 H7MB,H7MC), C7N(H7NA,H7NB,H7NC), C8M(H8MA,H8MB,H8MC)
;
_olex2_submission_special_instructions 'No special instructions were received'