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_7706136
_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                 114.211(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.846(7)
_cell_length_b                   19.201(5)
_cell_length_c                   32.426(7)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    240
_cell_measurement_theta_max      25.54
_cell_measurement_theta_min      2.46
_cell_volume                     16380(7)
_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      240
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47150
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.384
_diffrn_source_current           22.0
_diffrn_source_power             0.99
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.142
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1159 before and 0.0635 after correction. The Ratio of minimum to maximum transmission is 0.6193. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             7668
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         14428
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0147P)^2^+511.2505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10219
_reflns_number_total             14428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03340e2.cif
_cod_data_source_block           3HT
_cod_original_cell_volume        16381(7)
_cod_database_code               7706136
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.411
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Shared sites
{Re3, W3}
{Re1, W1}
{Re2, W2}
3. Restrained distances
 O6M-H6M
 0.85 with sigma of 0.01
 C13S-O13S
 1.4 with sigma of 0.02
 O13S-C13S
 1.4 with sigma of 0.02
 O5M-H5M
 0.85 with sigma of 0.01
 O7M-C7M
 1.4 with sigma of 0.02
 C7N-O7M
 1.4 with sigma of 0.02
 O10M-H10M
 0.85 with sigma of 0.01
 O11M-H11M
 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
 O8M-H8M
 0.85 with sigma of 0.01
 O9M-H9M
 0.85 with sigma of 0.01
 C16S-O16S
 1.4 with sigma of 0.02
 O2S-C2S
 1.4 with sigma of 0.02
 O3S-C3S
 1.4 with sigma of 0.02
 O11S-C11S
 1.4 with sigma of 0.02
 C10S-O10S
 1.4 with sigma of 0.02
 O9S-C9S
 1.4 with sigma of 0.02
 C15S-O15S
 1.4 with sigma of 0.02
 O5S-C5S
 1.4 with sigma of 0.02
 C12M-O12M
 1.4 with sigma of 0.02
 O12M-C12N
 1.4 with sigma of 0.02
 O12M-H12A
 0.85 with sigma of 0.01
 O12M-H12M
 0.85 with sigma of 0.01
 C4M-O4M
 1.4 with sigma of 0.02
 C4N-O4M
 1.4 with sigma of 0.02
 O4M-H4M
 0.85 with sigma of 0.01
 O4M-H4MA
 0.85 with sigma of 0.01
 O14S-C14S
 1.4 with sigma of 0.02
 C12S_$1-O12S_$1
 1.4 with sigma of 0.02
 O4S_$1-C4S_$1
 1.4 with sigma of 0.02
 C8S_$2-O8S_$2
 1.4 with sigma of 0.02
 C7S-O7S
 1.4 with sigma of 0.02
 O13S-O7M
 3.3 with sigma of 0.02
 O7M-H7MA
 0.86 with sigma of 0.01
 O7M-H7M
 0.86 with sigma of 0.01
 H7M-O13S
 2.58 with sigma of 0.02
 C6M-H6M
 1.858068 with sigma of 0.02
 Fe3-H6M
 2.690204 with sigma of 0.02
 C5M-H5M
 1.865076 with sigma of 0.02
 Fe3-H5M
 2.631727 with sigma of 0.02
 C10M-H10M
 1.916783 with sigma of 0.02
 Fe5-H10M
 2.698926 with sigma of 0.02
 C11M-H11M
 1.872267 with sigma of 0.02
 Fe5-H11M
 2.717876 with sigma of 0.02
 C3M-H3M
 1.893816 with sigma of 0.02
 Fe2-H3M
 2.686361 with sigma of 0.02
 C2M-H2M
 1.938204 with sigma of 0.02
 Fe2-H2M
 2.767683 with sigma of 0.02
 C1M-H1M
 1.891701 with sigma of 0.02
 Fe2-H1M
 2.71393 with sigma of 0.02
 C8M-H8M
 1.901447 with sigma of 0.02
 Fe4-H8M
 2.700932 with sigma of 0.02
 C9M-H9M
 1.920707 with sigma of 0.02
 Fe4-H9M
 2.780562 with sigma of 0.02
 C12N-H12A
 1.849796 with sigma of 0.02
 Fe5-H12A
 2.635335 with sigma of 0.02
 C12M-H12M
 1.86479 with sigma of 0.02
 Fe5-H12M
 2.690013 with sigma of 0.02
 C4M-H4M
 1.846172 with sigma of 0.02
 Fe3-H4M
 2.702618 with sigma of 0.02
 C4N-H4MA
 1.85586 with sigma of 0.02
 Fe3-H4MA
 2.718472 with sigma of 0.02
 H9M_$1-C12S_$1
 1.87 with sigma of 0.04
 H5MB-O8S
 1.87 with sigma of 0.04
 C7M-H7M
 1.859822 with sigma of 0.02
 Fe4-H7M
 2.764684 with sigma of 0.02
 Fe4-H7MA
 2.774412 with sigma of 0.02
 C7N-H7MA
 1.874925 with sigma of 0.02
4. Rigid bond restraints
 O9M, C9M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within
1.7A
O9M \\sim C9M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O5M \\sim C5M: 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
0.02 within 3A
O12M \\sim C12M \\sim C12N: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
Uanis(C4) \\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 0.01
Uanis(N7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(Re1) = Uanis(W1)
Uanis(Re2) = Uanis(W2)
Uanis(W2) = Uanis(Re2)
Uanis(W1) = Uanis(Re1)
Uanis(Re3) = Uanis(W3)
6. Others
 Fixed Sof: Re1(0.5) Re2(0.5) Re3(0.5) W1(0.5) W2(0.5) W3(0.5) H4M(0.65)
 H4MA(0.35) H7M(0.5) H7MA(0.5) H12A(0.5) H12M(0.5) C4M(0.65) H4MB(0.65)
 H4MC(0.65) H4MD(0.65) C7M(0.5) H7MB(0.5) H7MC(0.5) H7MD(0.5) C12M(0.5)
 H12B(0.5) H12C(0.5) H12D(0.5) C4N(0.35) H4NA(0.35) H4NB(0.35) H4NC(0.35)
 C7N(0.5) H7NA(0.5) H7NB(0.5) H7NC(0.5) C12N(0.5) H12E(0.5) H12F(0.5) H12G(0.5)
 O1S(0.5) C1S(0.5) O2S(0.5) C2S(0.5) O3S(0.25) C3S(0.25) O4S(0.125) C4S(0.125)
 O5S(0.5) C5S(0.5) O6S(0.5) C6S(0.5) O7S(0.25) C7S(0.25) O8S(0.125) C8S(0.125)
 O9S(0.125) C9S(0.125) O10S(0.25) C10S(0.25) O11S(0.25) C11S(0.25) O12S(0.125)
 C12S(0.125) O13S(0.25) C13S(0.25) O14S(0.25) C14S(0.25) O15S(0.25) C15S(0.25)
 O16S(0.25) C16S(0.25) O17S(0.25) C17S(0.25) O18S(0.25) C18S(0.25)
7.a Idealised Me refined as rotating group:
 C1M(H1MA,H1MB,H1MC), C2M(H2MA,H2MB,H2MC), C3M(H3MA,H3MB,H3MC), C4M(H4MB,H4MC,
 H4MD), C5M(H5MA,H5MB,H5MC), 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), C4N(H4NA,H4NB,H4NC), C7N(H7NA,H7NB,H7NC), C12N(H12E,H12F,
 H12G)
;
_shelx_res_checksum              97697
_olex2_submission_special_instructions 'No special instructions were received'