Cluster dynamics of heterometallic trinuclear clusters during ligand substitution, redox chemistry, and group transfer processes.
Juda, Cristin E.; Handford, Rex C.; Bartholomew, Amymarie K.; Powers, Tamara M.; Gu, Nina X.; Meyer, Elisabeth; Roth, Nikolaj; Chen, Yu-Sheng; Zheng, Shao-Liang; Betley, Theodore A.; Chemical science 15 (2024) 8242–8248; doi:10.1039/d3sc03606e

data_1571003
_publ_section_title
;
 Cluster dynamics of heterometallic trinuclear clusters during ligand
 substitution, redox chemistry, and group transfer processes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8242
_journal_page_last               8248
_journal_paper_doi               10.1039/d3sc03606e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C54 H94.96 Fe2 N6 Na2 O3 Si3'
_chemical_formula_sum            'C54 H94.96 Fe2 N6 Na2 O3 Si3'
_chemical_formula_weight         1118.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                106.479(4)
_cell_angle_beta                 93.058(4)
_cell_angle_gamma                106.770(4)
_cell_formula_units_Z            2
_cell_length_a                   11.040(2)
_cell_length_b                   14.175(3)
_cell_length_c                   21.290(5)
_cell_measurement_reflns_used    6644
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.627
_cell_measurement_theta_min      2.321
_cell_volume                     3025.6(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX v2016.1.0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.975
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25978
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.709
_diffrn_reflns_theta_min         1.580
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0457 before and 0.0412 after correction.
The Ratio of minimum to maximum transmission is 0.9344.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         11243
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0386P)^2^+0.9818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8451
_reflns_number_total             11243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03606e2.cif
_cod_data_source_block           46work1_a
_cod_depositor_comments
'Adding full bibliography for 1571003--1571015.cif.'
_cod_database_code               1571003
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C01V) = Uanis(C0AA)
Uanis(C01R) = Uanis(C2)
Uanis(C01Z) = Uanis(C1)
Uanis(C01I) = Uanis(C1AA)
Uanis(Si05) = Uanis(Si)
Uanis(C01M) = Uanis(C2AA)
Uanis(C01O) = Uanis(C3AA)
Uanis(C01T) = Uanis(C4AA)
Uanis(C01E) = Uanis(C5AA)
Uanis(C01G) = Uanis(C6AA)
Uanis(C01B) = Uanis(C7AA)
Uanis(O00G) = Uanis(O00H)
Uanis(C01S) = Uanis(C8AA)
Uanis(C01W) = Uanis(C9AA)
Uanis(C01L) = Uanis(C0BA)
Uanis(C01X) = Uanis(C01Y)
Uanis(O00E) = Uanis(O00F)
Uanis(C01Q) = Uanis(C1BA)
Uanis(C01P) = Uanis(C2BA)
Uanis(C01K) = Uanis(C3BA)
Uanis(C01U) = Uanis(C4BA)
3. Same fragment restrains
{C01I, C01R, C01Z, C01V} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1AA, C1, C2, C0AA}
4. Others
 Sof(C1AA)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(1)
 Sof(C01I)=Sof(C01R)=Sof(H01V)=Sof(H01W)=Sof(H01X)=Sof(C01Z)=Sof(H01Y)=Sof(H)=
 Sof(HA)=Sof(C01V)=Sof(H01Z)=Sof(HB)=Sof(HC)=FVAR(1)
 Sof(Si)=Sof(C2AA)=Sof(C3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=Sof(C4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(H4AD)=Sof(C5AA)=Sof(H5AB)=Sof(H5AC)=Sof(H5AD)=Sof(C6AA)=
 Sof(H6AB)=Sof(H6AC)=Sof(H6AD)=Sof(C7AA)=Sof(H7AB)=Sof(H7AC)=Sof(H7AD)=1-FVAR(2)
 Sof(Si05)=Sof(C01B)=Sof(H01B)=Sof(H01C)=Sof(H01D)=Sof(C01E)=Sof(H01E)=
 Sof(H01F)=Sof(H01G)=Sof(C01G)=Sof(H01P)=Sof(H01Q)=Sof(H01R)=Sof(C01M)=
 Sof(C01O)=Sof(H4AA)=Sof(HL)=Sof(HM)=Sof(C01T)=Sof(H8AA)=Sof(HQ)=Sof(HR)=FVAR(2)
 Sof(O00H)=Sof(C8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9AA)=Sof(H9AB)=Sof(C0BA)=
 Sof(H0BB)=Sof(C01Y)=Sof(H8BA)=Sof(H6CA)=Sof(H7CA)=1-FVAR(3)
 Sof(O00G)=Sof(C01L)=Sof(H2AA)=Sof(HH)=Sof(HI)=Sof(C01S)=Sof(H7AA)=Sof(HP)=
 Sof(C01W)=Sof(H0BA)=Sof(HU)=Sof(C01X)=Sof(H1BA)=Sof(HV)=Sof(HW)=FVAR(3)
 Sof(O00F)=Sof(C1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2BA)=Sof(H2BB)=Sof(H2BC)=
 Sof(C3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C4BA)=Sof(H4BB)=Sof(H4BC)=1-FVAR(4)
 Sof(O00E)=Sof(C01K)=Sof(H1AA)=Sof(HF)=Sof(HG)=Sof(C01P)=Sof(H5AA)=Sof(HN)=
 Sof(C01Q)=Sof(H6AA)=Sof(HO)=Sof(C01U)=Sof(H9AA)=Sof(HS)=Sof(HT)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00T(H00T), C014(H014)
5.b Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00U(H00C,H00D), C01F(H01N,H01O), C01P(H5AA,HN), C01Q(H6AA,
 HO), C01S(H7AA,HP), C01W(H0BA,HU), C011(H2BA,HX), C016(H5BA,H1CA), C8AA(H8AB,
 H8AC), C1BA(H1BB,H1BC), C2BA(H2BB,H2BC), C3BA(H3BB,H3BC), C4BA(H4BB,H4BC)
5.c Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00Q(H00Q), C00S(H00S), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C01A(H01A), C010(H010), C015(H015), C017(H017),
 C9AA(H9AB)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C0AA(H0AA,H0AB,H0AC), C01B(H01B,H01C,H01D),
 C01E(H01E,H01F,H01G), C01C(H01H,H01I,H01J), C01D(H01K,H01L,H01M), C01G(H01P,
 H01Q,H01R), C01H(H01S,H01T,H01U), C01R(H01V,H01W,H01X), C01Z(H01Y,H,HA),
 C01V(H01Z,HB,HC), C01J(H01,HD,HE), C01K(H1AA,HF,HG), C01L(H2AA,HH,HI),
 C01N(H3AA,HJ,HK), C01O(H4AA,HL,HM), C01T(H8AA,HQ,HR), C01U(H9AA,HS,HT),
 C01X(H1BA,HV,HW), C3AA(H3AB,H3AC,H3AD), C4AA(H4AB,H4AC,H4AD), C5AA(H5AB,H5AC,
 H5AD), C6AA(H6AB,H6AC,H6AD), C7AA(H7AB,H7AC,H7AD), C012(H3BA,HY,HZ), C013(H4BA,
 H9BA,H0CA), C018(H6BA,H2CA,H3CA), C019(H7BA,H4CA,H5CA), C01Y(H8BA,H6CA,H7CA)
5.e :
 C0BA(H0BB)
;
_shelx_res_checksum              15062
_olex2_submission_special_instructions 'No special instructions were received'