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_7706133
_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 Re5 W'
_chemical_formula_weight         3955.88
_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                 113.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.6620(17)
_cell_length_b                   19.4695(10)
_cell_length_c                   32.620(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.41
_cell_volume                     16648(2)
_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 0.899
_diffrn_measured_fraction_theta_max 0.899
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            22624
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.412
_diffrn_source_current           22.0
_diffrn_source_power             0.99
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0354 after correction.
The Ratio of minimum to maximum transmission is 0.6194.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             7676
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.437
_refine_diff_density_min         -2.167
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         13236
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0460P)^2^+501.2677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10434
_reflns_number_total             13236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03340e2.cif
_cod_data_source_block           1RT
_cod_original_cell_volume        16648.0(18)
_cod_database_code               7706133
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.412
_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
 C5M-O5M
 1.4 with sigma of 0.02
 O12M-C12N
 1.4 with sigma of 0.02
 C5S-O5S
 1.4 with sigma of 0.02
 O12M-C12M
 1.4 with sigma of 0.01
 O12M-H12A
 0.85 with sigma of 0.01
 O12M-H12M
 0.85 with sigma of 0.01
 O7M-C7N
 1.4 with sigma of 0.02
 C7M-O7M
 1.4 with sigma of 0.02
 O7M-H7MA
 0.85 with sigma of 0.01
 C4M-O4M
 1.4 with sigma of 0.02
 C1S-O1SA
 1.4 with sigma of 0.02
 O7M-H7M
 0.85 with sigma of 0.01
 O1SA_$2-H7MA
 2.5 with sigma of 0.02
 O4M-C4M
 1.4 with sigma of 0.01
 H4MC_$1-H4MC
 -3.2 with sigma of 0.02
 C5N-O5M
 1.4 with sigma of 0.02
 O9M-C9M
 1.4 with sigma of 0.02
 C1M-O1M
 1.4 with sigma of 0.01
 O9S-C9S
 1.4 with sigma of 0.02
 H1M-Fe2
 2.67 with sigma of 0.02
 H1M-O9S
 -2 with sigma of 0.02
 O8S-C8S
 1.4 with sigma of 0.02
 O10S-C10S
 1.4 with sigma of 0.02
 C2S-O2SA
 1.4 with sigma of 0.02
 C12S-O12S
 1.4 with sigma of 0.02
 O11S-C11S
 1.4 with sigma of 0.02
 C6S-O6S
 1.4 with sigma of 0.02
 C26-O7S
 1.4 with sigma of 0.02
 C4S-O4S
 1.4 with sigma of 0.02
 O2SB-C2S
 1.4 with sigma of 0.02
 O2SA-C2S
 1.4 with sigma of 0.02
 O1SB-C1S
 1.4 with sigma of 0.02
 O11M-H11M
 0.85 with sigma of 0.01
 O3M-H3M
 0.85 with sigma of 0.01
 O8M-H8M
 0.85 with sigma of 0.01
 O5M-H5M
 0.85 with sigma of 0.01
 O5M-H5MA
 0.85 with sigma of 0.01
 O4M-H4M
 0.85 with sigma of 0.01
 H2M-Fe2
 2.67 with sigma of 0.02
 O9M-H9M
 0.85 with sigma of 0.01
 C12M-H12M
 1.859083 with sigma of 0.02
 Fe5-H12M
 2.615053 with sigma of 0.02
 C12N-H12A
 1.870196 with sigma of 0.02
 Fe5-H12A
 2.766853 with sigma of 0.02
 C7N-H7MA
 1.876842 with sigma of 0.02
 Fe4-H7M
 2.730652 with sigma of 0.02
 C7M-H7M
 1.861441 with sigma of 0.02
 Fe4-H7MA
 2.735242 with sigma of 0.02
 C4M-H4M
 1.854942 with sigma of 0.02
 C9M-H9M
 1.873946 with sigma of 0.02
 C5N-H5MA
 1.86081 with sigma of 0.02
 Fe2-H3M
 2.692643 with sigma of 0.02
 C8M-H8M
 1.884236 with sigma of 0.02
 C3M-H3M
 1.879578 with sigma of 0.02
 C11M-H11M
 1.854114 with sigma of 0.02
 Fe3-H5M
 2.702735 with sigma of 0.02
 Fe5-H11M
 2.711022 with sigma of 0.02
 C5M-H5M
 1.861406 with sigma of 0.02
 Fe3-H5MA
 2.613647 with sigma of 0.02
 Fe4-H8M
 2.729079 with sigma of 0.02
 Fe3-H4M
 2.657208 with sigma of 0.02
 Fe4-H9M
 2.749849 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C12M \\sim O12M: within 3A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3A
O12M \\sim C12N: within 3A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3A
C7M \\sim O7M: within 3A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3A
C7N \\sim O7M: within 3A with sigma of 0.02 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
C1M \\sim O1M: within 3A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3A
O5M \\sim C5N: 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
Uanis(C9M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(N6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(N16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C12N) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C12M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C5M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(N15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(N8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(Re3) = Uanis(W3)
Uanis(Re1) = Uanis(W1)
Uanis(Re2) = Uanis(W2)
5. Others
 Fixed Sof: Re1(0.83333) Re2(0.83333) Re3(0.83333) H5M(0.6) H5MA(0.4) H7M(0.5)
 H7MA(0.5) H12M(0.7) H12A(0.3) C5M(0.6) H5MB(0.6) H5MC(0.6) H5MD(0.6) C7M(0.5)
 H7MB(0.5) H7MC(0.5) H7MD(0.5) C7N(0.5) H7NA(0.5) H7NB(0.5) H7NC(0.5)
 O11S(0.25) C11S(0.25) O3S(0.5) C3S(0.5) C5N(0.4) H5NA(0.4) H5NB(0.4) H5NC(0.4)
 C12M(0.7) H12B(0.7) H12C(0.7) H12D(0.7) C12N(0.3) H12E(0.3) H12F(0.3)
 H12G(0.3) O10S(0.5) C10S(0.5) O5S(0.25) C5S(0.25) O9S(0.5) C9S(0.5) O2SA(0.25)
 C2S(0.5) O1SA(0.25) C1S(0.5) O12S(0.25) C12S(0.25) O6S(0.25) C6S(0.25)
 C26(0.25) O7S(0.25) C4S(0.25) O4S(0.25) O2SB(0.25) O1SB(0.25) W3(0.16667)
 W1(0.16667) W2(0.16667)
6.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), C10M(H10A,H10B,H10C), C11M(H11A,H11B,H11C), C7N(H7NA,H7NB,H7NC),
 C5N(H5NA,H5NB,H5NC), C12M(H12B,H12C,H12D), C12N(H12E,H12F,H12G), C9M(H9MA,H9MB,
 H9MC)
6.b Idealised tetrahedral OH refined as rotating group:
 O1M(H1M), O2M(H2M), O6M(H6M), O10M(H10M)
;
_shelx_res_checksum              53462
_olex2_submission_special_instructions 'No special instructions were received'