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_7126426
_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 Fe3 N12, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H54 Fe3 N12 O2'
_chemical_formula_weight         1190.74
_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             2018-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2020-04-18 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.485(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.719(7)
_cell_length_b                   22.281(13)
_cell_length_c                   20.337(12)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.18
_cell_volume                     5308(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART CCD APEX2 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD APEX2 area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1618
_diffrn_reflns_av_unetI/netI     0.1425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.479
_diffrn_reflns_theta_min         1.356
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0814 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.8666.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         10904
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5709
_reflns_number_total             10904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02346a2.cif
_cod_data_source_block           Fe3TPM2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126426--7126428.cif.
;
_cod_original_cell_volume        5309(5)
_cod_database_code               7126426
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O2S-C5S \\sim O2T-C5T
 with sigma of 0.02
 C5S-C6S \\sim C5T-C6T
 with sigma of 0.02
 C6S-C7S \\sim C6T-C7T
 with sigma of 0.02
 C7S-C8S \\sim C7T-C8T
 with sigma of 0.02
 C8S-O2S \\sim C8T-O2T
 with sigma of 0.02
3. Rigid bond restraints
 O2S, C5S, C6S, C7S, C8S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2S \\sim C5S \\sim C6S \\sim C7S \\sim C8S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O2S) = Uanis(O2T)
Uanis(C5S) = Uanis(C5T)
Uanis(C6S) = Uanis(C6T)
Uanis(C7S) = Uanis(C7T)
Uanis(C8S) = Uanis(C8T)
5. Others
 Sof(O2T)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=Sof(C6T)=Sof(H6TA)=Sof(H6TB)=Sof(C7T)=
 Sof(H7TA)=Sof(H7TB)=Sof(C8T)=Sof(H8TA)=Sof(H8TB)=1-FVAR(1)
 Sof(O2S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(C7S)=
 Sof(H7SA)=Sof(H7SB)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C38(H38)
6.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,
 H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB), C5T(H5TA,H5TB),
 C6T(H6TA,H6TB), C7T(H7TA,H7TB), C8T(H8TA,H8TB)
6.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D), C5(H5), C6(H6), C7(H7), C8(H8),
 C11(H11), C12(H12), C16(H16), C17(H17), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35),
 C36(H36), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49),
  C50(H50), C53(H53), C54(H54), C55(H55), C56(H56)
;
_shelx_res_checksum              64835
_olex2_submission_special_instructions 'No special instructions were received'