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_7706140
_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                 113.4990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.5946(8)
_cell_length_b                   19.2126(5)
_cell_length_c                   32.3269(9)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.56
_cell_volume                     16286.8(8)
_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      100
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_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            75376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.398
_diffrn_source_current           22.0
_diffrn_source_power             0.99
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.104
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1042 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.7394. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             8020
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.162
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         14387
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0284P)^2^+199.9907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12033
_reflns_number_total             14387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03340e2.cif
_cod_data_source_block           5LT
_cod_database_code               7706140
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.400
_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
{Re1, W1}
{Re2, W2}
{Re3, W3}
3. Restrained distances
 O7M-C7M
 1.4 with sigma of 0.02
 C13S-O13S
 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
 C7N-O7M
 1.4 with sigma of 0.02
 C5S-O5S
 1.4 with sigma of 0.02
 C9S-O9S
 1.4 with sigma of 0.02
 O1SB-C1S
 1.4 with sigma of 0.02
 H4MA-O13S_$1
 2 with sigma of 0.02
 O3S-C3S
 1.4 with sigma of 0.02
 C11S-O11S
 1.4 with sigma of 0.02
 O14S-C14S
 1.4 with sigma of 0.02
 C2S-O2S
 1.4 with sigma of 0.02
 C8S-O8S
 1.4 with sigma of 0.02
 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
 O10M-H10M
 0.85 with sigma of 0.01
 O11M-H11M
 0.85 with sigma of 0.01
 O6M-H6M
 0.85 with sigma of 0.01
 O8M-H8M
 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
 O9M-H9M
 0.85 with sigma of 0.01
 C7S-O7S
 1.4 with sigma of 0.02
 C6S-O6S
 1.4 with sigma of 0.02
 C5O-O5M
 1.4 with sigma of 0.02
 C5N-O5M
 1.4 with sigma of 0.02
 O16S-C16S
 1.4 with sigma of 0.02
 O1SA-C1S
 1.4 with sigma of 0.02
 O5M-H5MB
 0.87 with sigma of 0.01
 C12M-O12M
 1.4 with sigma of 0.02
 O10S-C10S
 1.4 with sigma of 0.02
 H12M-O12M
 0.85 with sigma of 0.02
 H5MA-O5M
 0.85 with sigma of 0.02
 H5M-O5M
 0.85 with sigma of 0.02
 O4S-C4S
 1.4 with sigma of 0.02
 C15S-O15S
 1.4 with sigma of 0.02
 C5M-O5M
 1.4 with sigma of 0.02
 C15A-Re2
 2.13 with sigma of 0.02
 Re2-C15B
 2.13 with sigma of 0.02
 C16A-Re2
 2.13 with sigma of 0.02
 C16B-Re2
 2.13 with sigma of 0.02
 C4M-H4M
 1.850555 with sigma of 0.02
 Fe3-H4M
 2.703835 with sigma of 0.02
 C4N-H4MA
 1.918357 with sigma of 0.02
 Fe3-H4MA
 2.741848 with sigma of 0.02
 C3M-H3M
 1.912633 with sigma of 0.02
 Fe2-H3M
 2.687356 with sigma of 0.02
 C2M-H2M
 1.891219 with sigma of 0.02
 Fe2-H2M
 2.742154 with sigma of 0.02
 C1M-H1M
 1.90549 with sigma of 0.02
 Fe2-H1M
 2.702069 with sigma of 0.02
 C10M-H10M
 1.89647 with sigma of 0.02
 Fe5-H10M
 2.680846 with sigma of 0.02
 C11M-H11M
 1.880003 with sigma of 0.02
 Fe5-H11M
 2.711672 with sigma of 0.02
 C6M-H6M
 1.870243 with sigma of 0.02
 Fe3-H6M
 2.661203 with sigma of 0.02
 C8M-H8M
 1.881713 with sigma of 0.02
 Fe4-H8M
 2.692691 with sigma of 0.02
 C7N-H7MA
 1.898861 with sigma of 0.02
 Fe4-H7MA
 2.752477 with sigma of 0.02
 C7M-H7M
 1.898284 with sigma of 0.02
 Fe4-H7M
 2.788086 with sigma of 0.02
 C9M-H9M
 1.924594 with sigma of 0.02
 Fe4-H9M
 2.767234 with sigma of 0.02
 C5O-H5MB
 1.904549 with sigma of 0.02
 Fe3-H5MB
 2.764044 with sigma of 0.02
 H12M-Fe5
 2.67 with sigma of 0.04
 O2S-H12M
 1.87 with sigma of 0.04
 H5MA-C5N
 1.87 with sigma of 0.04
 H5MA-Fe3
 2.67 with sigma of 0.04
 H5M-Fe3
 2.67 with sigma of 0.04
 H12M-C12M
 1.87 with sigma of 0.04
 H12C-H12M
 2 with sigma of 0.04
 C5M-H5M
 1.87 with sigma of 0.04
4. Rigid bond restraints
 O4M, C4N
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O6M \\sim C6M: 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
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
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 0.02
Uanis(C15B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C5M) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(Re2) = Uanis(W2)
Uanis(Re3) = Uanis(W3)
Uanis(Re1) = Uanis(W1)
6. Others
 Fixed Sof: Re1(0.16667) Re2(0.16667) Re3(0.16667) W1(0.83333) W2(0.83333)
 W3(0.83333) H4M(0.5) H4MA(0.5) H5MB(0.3) H7M(0.5) H7MA(0.5) N15A(0.6)
 N16A(0.6) N15B(0.4) N16B(0.4) C15A(0.6) C16A(0.6) C15B(0.4) C16B(0.4) C4M(0.5)
 H4MB(0.5) H4MC(0.5) H4MD(0.5) C5M(0.3) H5MC(0.3) H5MD(0.3) H5ME(0.3) C7M(0.5)
 H7MB(0.5) H7MC(0.5) H7MD(0.5) C4N(0.5) H4NA(0.5) H4NB(0.5) H4NC(0.5) C5N(0.4)
 H5NA(0.4) H5NB(0.4) H5NC(0.4) C7N(0.5) H7NA(0.5) H7NB(0.5) H7NC(0.5) C5O(0.3)
 H5OA(0.3) H5OB(0.3) H5OC(0.3) O2S(0.5) C2S(0.5) O4S(0.25) C4S(0.25) O6S(0.5)
 C6S(0.5) O7S(0.5) C7S(0.5) O8S(0.5) C8S(0.5) O9S(0.5) C9S(0.5) O10S(0.25)
 C10S(0.25) H5M(0.3) H5MA(0.4) O11S(0.5) C11S(0.5) O12S(0.25) C12S(0.25)
 O13S(0.25) C13S(0.25) O14S(0.5) C14S(0.5) O15S(0.25) C15S(0.25) O16S(0.25)
 C16S(0.25) O1SA(0.25) O1SB(0.25) C1S(0.5)
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(H5MC,H5MD,H5ME), 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(H12A,H12B,H12C), C4N(H4NA,H4NB,H4NC), C5N(H5NA,H5NB,H5NC), C7N(H7NA,H7NB,
 H7NC), C5O(H5OA,H5OB,H5OC)
;
_shelx_res_checksum              22586
_olex2_submission_special_instructions 'No special instructions were received'