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_7706142
_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 Re1 W5, 15(C H3 O H)'
_chemical_formula_sum            'C87 H156 Fe9 N48 O39 Re W5'
_chemical_formula_weight         4106.69
_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                 113.6470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.820(2)
_cell_length_b                   19.5768(15)
_cell_length_c                   32.775(3)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.37
_cell_volume                     16939(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42878
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.375
_diffrn_source_current           22.0
_diffrn_source_power             0.99
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1051 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.7187.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             8020
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         14895
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0230P)^2^+314.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11776
_reflns_number_total             14895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03340e2.cif
_cod_data_source_block           5RT
_cod_original_cell_volume        16939(3)
_cod_database_code               7706142
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.547
_shelx_estimated_absorpt_t_min   0.238
_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
{W3, Re3}
{W2, Re2}
{W1, Re1}
3. Restrained distances
 O1S-C1SA
 1.4 with sigma of 0.02
 H12M-O12M
 0.85 with sigma of 0.01
 C12M-O12M
 1.42 with sigma of 0.01
 C12N-O12M
 1.4 with sigma of 0.02
 C5M-O5M
 1.4 with sigma of 0.02
 C5N-O5M
 1.4 with sigma of 0.02
 O12M-H12A
 0.85 with sigma of 0.01
 O5M-H5MA
 0.85 with sigma of 0.01
 O5M-H5M
 0.85 with sigma of 0.01
 O2M-H2M
 0.85 with sigma of 0.01
 O12S-C12S
 1.4 with sigma of 0.02
 O11S-C11S
 1.4 with sigma of 0.02
 O10S-C10S
 1.4 with sigma of 0.02
 C2S-O2S
 1.4 with sigma of 0.02
 O7S-C7S
 1.4 with sigma of 0.02
 C8S-O8S
 1.4 with sigma of 0.02
 O13S-C13S
 1.4 with sigma of 0.02
 O3S-C3S
 1.4 with sigma of 0.02
 O5S-C5S
 1.4 with sigma of 0.02
 C4S-O4S
 1.4 with sigma of 0.02
 O9S-C9S
 1.4 with sigma of 0.02
 O6S-C6S
 1.4 with sigma of 0.02
 O6M-H6M
 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
 O3M-H3M
 0.85 with sigma of 0.01
 H9M-O4S
 -2.1 with sigma of 0.02
 O12S-H2M
 -2.1 with sigma of 0.02
 O4M-C4M
 1.4 with sigma of 0.01
 O4M-H4M
 0.85 with sigma of 0.01
 O1M-H1M
 0.85 with sigma of 0.01
 O7M-H7MA
 0.85 with sigma of 0.01
 O7M-H7M
 0.85 with sigma of 0.01
 H7M-O5S
 2.8 with sigma of 0.02
 Fe5-H12M
 2.62 with sigma of 0.02
 C12N-H12A
 1.865413 with sigma of 0.02
 Fe5-H12A
 2.626778 with sigma of 0.02
 Fe3-H5MA
 2.620099 with sigma of 0.02
 C2M-H2M
 1.898052 with sigma of 0.02
 C5N-H5MA
 1.85 with sigma of 0.02
 Fe2-H2M
 2.689286 with sigma of 0.02
 Fe3-H5M
 2.710676 with sigma of 0.02
 C5M-H5M
 1.85 with sigma of 0.02
 Fe4-H8M
 2.715087 with sigma of 0.02
 Fe3-H6M
 2.685727 with sigma of 0.02
 C3M-H3M
 1.898052 with sigma of 0.02
 C6M-H6M
 1.864468 with sigma of 0.02
 C8M-H8M
 1.889063 with sigma of 0.02
 C9M-H9M
 1.915429 with sigma of 0.02
 Fe4-H9M
 2.746224 with sigma of 0.02
 Fe2-H3M
 2.689286 with sigma of 0.02
 H12M-C12M
 1.8 with sigma of 0.04
 C4M-H4M
 1.850676 with sigma of 0.02
 Fe3-H4M
 2.677254 with sigma of 0.02
 C1M-H1M
 1.850189 with sigma of 0.02
 Fe2-H1M
 2.687733 with sigma of 0.02
 Fe4-H7M
 2.739782 with sigma of 0.02
 C7M-H7M
 1.905179 with sigma of 0.02
 Fe4-H7MA
 2.735673 with sigma of 0.02
 C7N-H7MA
 1.883777 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C12M \\sim O12M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
C12N \\sim O12M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
C5N \\sim O5M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
C5M \\sim O5M: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C7N) \\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 0.1
Uanis(C7M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(N16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(N15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(W3) = Uanis(Re3)
Uanis(W2) = Uanis(Re2)
Uanis(W1) = Uanis(Re1)
5. Others
 Fixed Sof: W1(0.83333) W2(0.83333) W3(0.83333) H5M(0.75) H5MA(0.25) H7M(0.5)
 H7MA(0.5) H12A(0.25) C1SA(0.5) C7M(0.5) H7MB(0.5) H7MC(0.5) H7MD(0.5) C7N(0.5)
 H7NA(0.5) H7NB(0.5) H7NC(0.5) C12M(0.75) H12B(0.75) H12C(0.75) H12D(0.75)
 C5M(0.75) H5MB(0.75) H5MC(0.75) H5MD(0.75) O11S(0.75) C11S(0.75) O10S(0.5)
 C10S(0.5) O2S(0.25) C2S(0.25) O7S(0.75) C7S(0.75) C8S(0.5) O8S(0.5) O13S(0.5)
 C13S(0.5) O3S(0.5) C3S(0.5) C5S(0.5) O5S(0.5) C1SB(0.5) O4S(0.5) C4S(0.5)
 C12N(0.25) H12E(0.25) H12F(0.25) H12G(0.25) C9S(0.25) O9S(0.25) O6S(0.5)
 C6S(0.5) C5N(0.25) H5NA(0.25) H5NB(0.25) H5NC(0.25) H12M(0.75) Re2(0.16667)
 Re3(0.16667) Re1(0.16667)
6.a Idealised Me refined as rotating group:
 C1M(H1MA,H1MB,H1MC), C6M(H6MA,H6MB,H6MC), C10M(H10A,H10B,H10C), C3M(H3MA,H3MB,
 H3MC), C2M(H2MA,H2MB,H2MC), C4M(H4MA,H4MB,H4MC), C8M(H8MA,H8MB,H8MC), C7M(H7MB,
 H7MC,H7MD), C7N(H7NA,H7NB,H7NC), C12M(H12B,H12C,H12D), C11M(H11A,H11B,H11C),
 C9M(H9MA,H9MB,H9MC), C5M(H5MB,H5MC,H5MD), C12N(H12E,H12F,H12G), C5N(H5NA,H5NB,
 H5NC)
6.b Idealised tetrahedral OH refined as rotating group:
 O10M(H10M), O11M(H11M)
;
_shelx_res_checksum              31191
_olex2_submission_special_instructions 'No special instructions were received'