Tuning of the phase transition between site selective SCO and intermetallic ET in trimetallic magnetic cyanido-bridged clusters.
Kobylarczyk, Jedrzej; Liberka, Michal; Stanek, Jan J.; Sieklucka, Barbara; Podgajny, Robert; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17321–17330; doi:10.1039/d0dt03340e

data_7706143
_publ_section_title
;
 Tuning of the phase transition between site selective SCO and
 intermetallic ET in trimetallic magnetic cyanido-bridged clusters.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17321
_journal_page_last               17330
_journal_paper_doi               10.1039/d0dt03340e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C72 H96 Fe9 N48 O24 Re5 W1, 10(C H3 O H)'
_chemical_formula_sum            'C82 H136 Fe9 N48 O34 Re3 W3'
_chemical_formula_weight         3951.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-23 deposited with the CCDC.	2020-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.134(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.828(3)
_cell_length_b                   19.3983(19)
_cell_length_c                   32.625(4)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.38
_cell_volume                     16650(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0654
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            109986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.380
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.059
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1406 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.5478. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       prism
_exptl_crystal_F_000             7668
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         16384
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0215P)^2^+114.2656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13406
_reflns_number_total             16384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03340e2.cif
_cod_data_source_block           3RT
_cod_original_cell_volume        16649(3)
_cod_database_code               7706143
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.463
_shelx_estimated_absorpt_t_min   0.209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Shared sites
{Re3, W3}
{Re1, W1}
{Re2, W2}
3. Restrained distances
 O20S-C20S
 1.4 with sigma of 0.02
 C21S-O21S
 1.4 with sigma of 0.02
 O17S-C17S
 1.4 with sigma of 0.02
 C6S-O6S
 1.4 with sigma of 0.02
 O5S-C5S
 1.4 with sigma of 0.02
 C10S-O10S
 1.4 with sigma of 0.02
 O22S-C22S
 1.4 with sigma of 0.02
 O13S-C13S
 1.4 with sigma of 0.02
 O8S-C8S
 1.4 with sigma of 0.02
 C14S-O14S
 1.4 with sigma of 0.02
 O9S-C9S
 1.4 with sigma of 0.02
 C2S-O2S
 1.4 with sigma of 0.02
 C7S-O7S
 1.4 with sigma of 0.02
 O3S-C3S
 1.4 with sigma of 0.02
 C12S-O12S
 1.4 with sigma of 0.02
 C16S-O16S
 1.4 with sigma of 0.02
 O19S-C19S
 1.4 with sigma of 0.02
 O11S-C11S
 1.4 with sigma of 0.02
 C4S-O4S
 1.4 with sigma of 0.02
 O8M-H8M
 0.85 with sigma of 0.01
 O9M-H9M
 0.85 with sigma of 0.01
 O7M-H7M
 0.85 with sigma of 0.01
 O3M-H3M
 0.85 with sigma of 0.01
 O2M-H2M
 0.85 with sigma of 0.01
 O1M-H1M
 0.85 with sigma of 0.01
 O11M-H11M
 0.85 with sigma of 0.01
 O10M-H10M
 0.85 with sigma of 0.01
 H7MA-O7M
 0.85 with sigma of 0.02
 O18S-C18S
 1.4 with sigma of 0.02
 H6M-O6M
 0.85 with sigma of 0.02
 O4M-H4M
 0.85 with sigma of 0.02
 H5M-O5M
 0.85 with sigma of 0.02
 H12A-O12M
 0.85 with sigma of 0.02
 H12M-O12M
 0.85 with sigma of 0.02
 H5MA-O5M
 0.85 with sigma of 0.02
 C8M-H8M
 1.889605 with sigma of 0.02
 Fe4-H8M
 2.700124 with sigma of 0.02
 C9M-H9M
 1.915567 with sigma of 0.02
 Fe4-H9M
 2.757782 with sigma of 0.02
 C7M-H7M
 1.899213 with sigma of 0.02
 Fe4-H7M
 2.775078 with sigma of 0.02
 C3M-H3M
 1.876688 with sigma of 0.02
 Fe2-H3M
 2.687091 with sigma of 0.02
 C2M-H2M
 1.941556 with sigma of 0.02
 Fe2-H2M
 2.777627 with sigma of 0.02
 C1M-H1M
 1.904403 with sigma of 0.02
 Fe2-H1M
 2.686089 with sigma of 0.02
 C11M-H11M
 1.878131 with sigma of 0.02
 Fe5-H11M
 2.724417 with sigma of 0.02
 C10M-H10M
 1.907154 with sigma of 0.02
 Fe5-H10M
 2.695194 with sigma of 0.02
 H7MA-Fe4
 2.67 with sigma of 0.04
 H7MA-C7N
 1.87 with sigma of 0.04
 H4M-C4M
 1.87 with sigma of 0.04
 H4M-Fe3
 2.67 with sigma of 0.04
 H5M-Fe3
 2.67 with sigma of 0.04
 H5M-C5M
 1.87 with sigma of 0.04
 H12A-Fe5
 2.67 with sigma of 0.04
 H12A-C12N
 1.87 with sigma of 0.04
 H12M-C12M
 1.87 with sigma of 0.04
 H12M-Fe5
 2.67 with sigma of 0.04
 H5MA-C5N
 1.83 with sigma of 0.04
 H5MA-Fe3
 2.6 with sigma of 0.04
4. Rigid bond restraints
 O12M, C12M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O12M \\sim C12N: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O12M \\sim C12M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O9M \\sim C9M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O1M \\sim C1M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.04 within 3A
O4M \\sim C4M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O5M \\sim C5M \\sim C5N: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
Uanis(C1M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(N16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C12M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C6M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(Re3) = Uanis(W3)
Uanis(Re2) = Uanis(W2)
Uanis(W2) = Uanis(Re2)
Uanis(W3) = Uanis(Re3)
Uanis(Re1) = Uanis(W1)
6. Others
 Fixed Sof: Re1(0.5) Re2(0.5) Re3(0.5) W1(0.5) W2(0.5) W3(0.5) H7M(0.65)
 H7MA(0.35) C5M(0.5) H5MB(0.5) H5MC(0.5) H5MD(0.5) C7M(0.65) H7MB(0.65)
 H7MC(0.65) H7MD(0.65) C12M(0.35) H12B(0.35) H12C(0.35) H12D(0.35) C5N(0.5)
 H5NA(0.5) H5NB(0.5) H5NC(0.5) C7N(0.35) H7NA(0.35) H7NB(0.35) H7NC(0.35)
 C12N(0.65) H12E(0.65) H12F(0.65) H12G(0.65) O2S(0.25) C2S(0.25) O3S(0.125)
 C3S(0.125) O4S(0.125) C4S(0.125) O5S(0.25) C5S(0.25) O6S(0.25) C6S(0.25)
 O7S(0.125) C7S(0.125) O8S(0.25) C8S(0.25) O9S(0.125) C9S(0.125) O10S(0.25)
 C10S(0.25) O11S(0.125) C11S(0.125) O12S(0.125) C12S(0.125) O13S(0.25)
 C13S(0.25) O14S(0.25) C14S(0.25) O15S(0.5) C15S(0.5) O16S(0.125) C16S(0.125)
 O17S(0.25) C17S(0.25) O18S(0.125) C18S(0.125) H5M(0.5) H5MA(0.5) H12A(0.65)
 H12M(0.35) O19S(0.125) C19S(0.125) O20S(0.5) C20S(0.5) O21S(0.25) C21S(0.25)
 O22S(0.25) C22S(0.25) O1SA(0.25) O1SB(0.125) C1S(0.375)
7.a Idealised Me refined as rotating group:
 C1M(H1MA,H1MB,H1MC), C2M(H2MA,H2MB,H2MC), C3M(H3MA,H3MB,H3MC), C4M(H4MA,H4MB,
 H4MC), C5M(H5MB,H5MC,H5MD), C6M(H6MA,H6MB,H6MC), C7M(H7MB,H7MC,H7MD), C8M(H8MA,
 H8MB,H8MC), C9M(H9MA,H9MB,H9MC), C10M(H10A,H10B,H10C), C11M(H11A,H11B,H11C),
 C12M(H12B,H12C,H12D), C5N(H5NA,H5NB,H5NC), C7N(H7NA,H7NB,H7NC), C12N(H12E,H12F,
 H12G)
;
_shelx_res_checksum              7164
_olex2_submission_special_instructions 'No special instructions were received'