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_7701980
_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         'C200 H216 Mn9 N64 O8 W6, 13(C O), C6 H14 O'
_chemical_formula_sum            'C219 H230 Mn9 N64 O22 W6'
_chemical_formula_weight         5708.22
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-27
_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                93.7930(10)
_cell_angle_beta                 98.1180(10)
_cell_angle_gamma                96.5350(10)
_cell_formula_units_Z            1
_cell_length_a                   20.2710(13)
_cell_length_b                   20.3406(13)
_cell_length_c                   20.3665(13)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.66
_cell_volume                     8230.5(9)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0694
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            97439
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.295
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0832 before and 0.0541 after correction. The Ratio of minimum to maximum transmission is 0.7418. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             2837
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.249
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1654
_refine_ls_number_reflns         29042
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+38.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20733
_reflns_number_total             29042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03903a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7701980--7701982.cif.'
_cod_database_code               7701980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.577
_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
2. Restrained distances
 C1S-O1S
 1.4 with sigma of 0.02
 C12S-C14S
 1.48 with sigma of 0.01
 C12S-C13S
 1.48 with sigma of 0.01
 C12S-O12S
 1.4 with sigma of 0.01
 O12S-C15S
 1.48 with sigma of 0.01
 C15S-C16S
 1.48 with sigma of 0.01
 C15S-O12S
 1.4 with sigma of 0.01
 C7S-O7S
 1.4 with sigma of 0.02
 O8S-C8S
 1.4 with sigma of 0.02
 C5S-O5S
 1.4 with sigma of 0.02
 O11S-H41A
 2.5 with sigma of 0.02
 C105_$1-C103_$1
 1.5 with sigma of 0.02
 C15S-C17S
 1.48 with sigma of 0.02
 C17S-C15S
 1.48 with sigma of 0.01
 C4S-O4S
 1.4 with sigma of 0.02
 H1MC-H10E_$1
 -2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C44B \\sim C43B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C43B \\sim C46B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C43B \\sim C45B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C12S \\sim C14S: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C14S \\sim C12S: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C52 \\sim C55B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C55B \\sim C53B \\sim C54B \\sim C52: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C105 \\sim C106 \\sim C103 \\sim C104: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C45A \\sim C43A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C17S \\sim C15S: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C1MA \\sim O1MA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C41B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C55B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C43B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C14S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C12S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C103) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(N40A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C40B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C1MA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: N40B(0.5) N40A(0.5) O12S(0.5) C40B(0.5) H40B(0.5) C43A(0.5)
 C57B(0.5) H57B(0.5) C40A(0.5) H40A(0.5) C47A(0.5) H47A(0.5) C57A(0.5)
 H57A(0.5) C49B(0.5) C11S(0.5) C47B(0.5) H47B(0.5) C55A(0.6) H55A(0.6)
 H55B(0.6) H55C(0.6) C49A(0.5) C48B(0.5) C50A(0.5) H50A(0.5) C42A(0.5)
 C56B(0.5) H56B(0.5) C48A(0.5) C50B(0.5) H50B(0.5) C54A(0.6) H54A(0.6)
 H54B(0.6) H54C(0.6) C41A(0.5) H41A(0.5) C44A(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) C46A(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C53A(0.6) H53A(0.6)
 H53B(0.6) H53C(0.6) C42B(0.5) C41B(0.5) H41B(0.5) C45A(0.5) H45A(0.5)
 H45B(0.5) H45C(0.5) C43B(0.5) C46B(0.5) H46D(0.5) H46E(0.5) H46F(0.5)
 C44B(0.5) H44D(0.5) H44E(0.5) H44F(0.5) C45B(0.5) H45D(0.5) H45E(0.5)
 H45F(0.5) C56A(0.5) H56A(0.5) O1MB(0.5) C1MB(0.5) H1MA(0.5) H1MB(0.5)
 H1MC(0.5) O1MA(0.5) O11S(0.5) C12S(0.5) H12S(0.5) C13S(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C14S(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C16S(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C17S(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
 C15S(0.5) H15S(0.5) C54B(0.4) H54D(0.4) H54E(0.4) H54F(0.4) C53B(0.4)
 H53D(0.4) H53E(0.4) H53F(0.4) C55B(0.4) H55D(0.4) H55E(0.4) H55F(0.4) O7S(0.5)
 O8S(0.5) C7S(0.5) C8S(0.5) O3S(0.25) C3S(0.25) O2S(0.25) C2S(0.25) O1S(0.25)
 C1S(0.25) O4S(0.25) C4S(0.25) C1MA(0.5) H1MD(0.5) H1ME(0.5) H1MF(0.5)
5.a Ternary CH refined with riding coordinates:
 C12S(H12S), C15S(H15S)
5.b Me refined with riding coordinates:
 C17S(H17A,H17B,H17C)
5.c Aromatic/amide H refined with riding coordinates:
 C117(H117), C100(H100), C80(H80), C77(H77), C110(H110), C60(H60), C67(H67),
 C97(H97), C87(H87), C116(H116), C76(H76), C61(H61), C70(H70), C90(H90),
 C96(H96), C81(H81), C107(H107), C101(H101), C40B(H40B), C57B(H57B), C40A(H40A),
  C47A(H47A), C57A(H57A), C47B(H47B), C50A(H50A), C56B(H56B), C50B(H50B),
 C41A(H41A), C41B(H41B), C56A(H56A)
5.d Idealised Me refined as rotating group:
 C3M(H3MA,H3MB,H3MC), C4M(H4MA,H4MB,H4MC), C65(H65A,H65B,H65C), C86(H86A,H86B,
 H86C), C66(H66A,H66B,H66C), C85(H85A,H85B,H85C), C2M(H2MA,H2MB,H2MC),
 C113(H11A,H11B,H11C), C64(H64A,H64B,H64C), C114(H11D,H11E,H11F), C73(H73A,H73B,
 H73C), C115(H11G,H11H,H11I), C94(H94A,H94B,H94C), C106(H10A,H10B,H10C),
 C84(H84A,H84B,H84C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C93(H93A,H93B,
 H93C), C105(H10D,H10E,H10F), C55A(H55A,H55B,H55C), C95(H95A,H95B,H95C),
 C54A(H54A,H54B,H54C), C104(H10G,H10H,H10I), C44A(H44A,H44B,H44C), C46A(H46A,
 H46B,H46C), C53A(H53A,H53B,H53C), C45A(H45A,H45B,H45C), C46B(H46D,H46E,H46F),
 C44B(H44D,H44E,H44F), C45B(H45D,H45E,H45F), C1MB(H1MA,H1MB,H1MC), C13S(H13A,
 H13B,H13C), C14S(H14A,H14B,H14C), C16S(H16A,H16B,H16C), C54B(H54D,H54E,H54F),
 C53B(H53D,H53E,H53F), C55B(H55D,H55E,H55F), C1MA(H1MD,H1ME,H1MF)
;
_shelx_res_checksum              934
_shelx_fab_checksum              28998
_olex2_submission_special_instructions 'No special instructions were received'