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_7126427
_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 N12 Zn3, 2(C4 H8 O), 0.18(H2 O)'
_chemical_formula_sum            'C64 H54.36 N12 O2.18 Zn3'
_chemical_formula_weight         1222.54
_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   mixed
_audit_creation_date             2020-01-29
_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                 92.1491(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5922(11)
_cell_length_b                   22.523(2)
_cell_length_c                   20.5743(19)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      65.067
_cell_measurement_theta_min      4.292
_cell_volume                     5368.0(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39654
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        65.123
_diffrn_reflns_theta_max         65.123
_diffrn_reflns_theta_min         2.910
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.4649
_exptl_absorpt_correction_T_min  0.3590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0683 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.7722. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             2519
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         9001
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0355P)^2^+8.4255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8416
_reflns_number_total             9001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02346a2.cif
_cod_data_source_block           Zn3TPM2
_cod_depositor_comments
'Adding full bibliography for 7126426--7126428.cif.'
_cod_original_cell_volume        5367.9(9)
_cod_database_code               7126427
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.810
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim O1T \\sim C2T \\sim C3T \\sim
C4T \\sim C5T: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O1S, C2S, C3S, C4S, C5S, O1T, C2T, C3T, C4T, C5T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Same fragment restrains
{O1S, C2S, C3S, C4S, C5S} sigma for 1-2: 0.01, 1-3: 0.04
as
{O1T, C2T, C3T, C4T, C5T}
5. Others
 Fixed Sof: O1S(0.82) C2S(0.82) H2SA(0.82) H2SB(0.82) C3S(0.82) H3SA(0.82)
 H3SB(0.82) C4S(0.82) H4SA(0.82) H4SB(0.82) C5S(0.82) H5SA(0.82) H5SB(0.82)
 O1T(0.18) C2T(0.18) H2TA(0.18) H2TB(0.18) C3T(0.18) H3TA(0.18) H3TB(0.18)
 C4T(0.18) H4TA(0.18) H4TB(0.18) C5T(0.18) H5TA(0.18) H5TB(0.18) O1W(0.18)
 H1WA(0.18) H1WB(0.18)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C19(H19), C20(H20)
6.c Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C2T(H2TA,
 H2TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB), C5T(H5TA,H5TB), C7S(H7SA,H7SB),
 C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10A,H10B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37),
 C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51), C54(H54), C55(H55)
;
_shelx_res_checksum              10968
_olex2_submission_special_instructions 'No special instructions were received'