Kinetic versus thermodynamic metalation enables synthesis of isostructural homo- and heterometallic trinuclear clusters.
Hyun, Sung-Min; Upadhyay, Apoorva; Das, Anuvab; Burns, Corey P.; Sung, Siyoung; Beaty, Jeremy D.; Bhuvanesh, Nattamai; Nippe, Michael; Powers, David C.; Chemical communications (Cambridge, England) 56 (2020) 5893–5896; doi:10.1039/d0cc02346a

data_7126428
_publ_section_title
;
 Kinetic versus thermodynamic metalation enables synthesis of
 isostructural homo- and heterometallic trinuclear clusters.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5893
_journal_page_last               5896
_journal_paper_doi               10.1039/d0cc02346a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C56 H38 Fe2 N12 Zn1, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H54 Fe2 N12 O2 Zn'
_chemical_formula_weight         1200.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-18 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.781(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6640(7)
_cell_length_b                   22.4568(14)
_cell_length_c                   20.4213(13)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      69.995
_cell_measurement_theta_min      3.792
_cell_volume                     5346.5(6)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            145466
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.174
_diffrn_reflns_theta_min         2.925
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.294
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.2650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0721 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.6899. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         10131
_refine_ls_number_restraints     440
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0327P)^2^+6.2165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10023
_reflns_number_total             10131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02346a2.cif
_cod_data_source_block           Fe2ZnTPM2
_cod_depositor_comments
'Adding full bibliography for 7126426--7126428.cif.'
_cod_database_code               7126428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.411
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
O6S \\sim C7S \\sim C8S \\sim C9S \\sim C10S \\sim O6T \\sim C7T \\sim C8T
\\sim C9T \\sim C10T: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.01
O1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim O1T \\sim C2T \\sim C3T \\sim
C4T \\sim C5T: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(Zn1) = Uanis(Fe1)
Uanis(Zn2) = Uanis(Fe2)
Uanis(Zn3) = Uanis(Fe3)
Uanis(O6T) = Uanis(O6S)
3. Rigid body (RIGU) restrains
 O6S, C7S, C8S, C9S, C10S, O6T, C7T, C8T, C9T, C10T
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1S, C2S, C3S, C4S, C5S, O1T, C2T, C3T, C4T, C5T
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Same fragment restrains
{O1S, C2S, C3S, C4S, C5S} sigma for 1-2: 0.005, 1-3: 0.04
as
{O1T, C2T, C3T, C4T, C5T}
{O6S, C7S, C8S, C9S, C10S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6T, C7T, C8T, C9T, C10T}
5. Others
 Sof(O6T)=Sof(C7T)=Sof(H7TA)=Sof(H7TB)=Sof(C8T)=Sof(H8TA)=Sof(H8TB)=Sof(C9T)=
 Sof(H9TA)=Sof(H9TB)=Sof(C10T)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(O6S)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(C9S)=
 Sof(H9SA)=Sof(H9SB)=Sof(C10S)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(O1T)=Sof(C2T)=Sof(H2TA)=Sof(H2TB)=Sof(C3T)=Sof(H3TA)=Sof(H3TB)=Sof(C4T)=
 Sof(H4TA)=Sof(H4TB)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=1-FVAR(2)
 Sof(O1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C4S)=
 Sof(H4SA)=Sof(H4SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=FVAR(2)
 Fixed Sof: Fe1(0.66666) Fe2(0.66666) Fe3(0.66666) Zn1(0.33333) Zn2(0.33333)
 Zn3(0.33333)
6.a Ternary CH refined with riding coordinates:
 C46(H46), C56(H56)
6.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C7S(H7SA,
 H7SB), C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10A,H10B), C2T(H2TA,H2TB),
 C3T(H3TA,H3TB), C4T(H4TA,H4TB), C5T(H5TA,H5TB), C7T(H7TA,H7TB), C8T(H8TA,H8TB),
  C9T(H9TA,H9TB), C10T(H10C,H10D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C47(H47), C48(H48),
  C49(H49), C50(H50), C53(H53), C54(H54)
;
_shelx_res_checksum              70175
_olex2_submission_special_instructions 'No special instructions were received'