Structural analysis and catalytic activity of tetranuclear metal carboxylate clusters with a [KZn3(μ3-OH)(OOCCPh3)6] or [Zn4(μ4-O)(OOCCPh3)6] central motif
Petrus, Rafał; Utko, Józef; Sobota, Piotr; New Journal of Chemistry 44 (2020) 13771–13780; doi:10.1039/D0NJ02540B

data_7059852
_publ_section_title
;
 Structural analysis and catalytic activity of tetranuclear metal
 carboxylate clusters with a [KZn3(\m3-OH)(OOCCPh3)6] or
 [Zn4(\m4-O)(OOCCPh3)6] central motif
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13771
_journal_page_last               13780
_journal_paper_doi               10.1039/D0NJ02540B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
' C122 H94 K N O13 Zn3, 0.2(C6 H14), 4(C2 H3 N) '
_chemical_formula_sum            'C131.2 H108.8 K N5 O13 Zn3'
_chemical_formula_weight         2198.64
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-04-14 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                74.68(3)
_cell_angle_beta                 84.79(3)
_cell_angle_gamma                66.28(3)
_cell_formula_units_Z            2
_cell_length_a                   14.302(4)
_cell_length_b                   15.362(5)
_cell_length_c                   27.872(9)
_cell_measurement_reflns_used    43615
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8013
_cell_measurement_theta_min      2.8888
_cell_volume                     5406(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'KUMA KM4 CCD \k-geometry diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            60695
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.067
_diffrn_reflns_theta_min         2.889
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         27833
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0767P)^2^+0.1918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22907
_reflns_number_total             27833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02540b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059852--7059854.cif.

 Adding full bibliography for 7059852--7059854.cif.
;
_cod_original_formula_sum        'C131.20 H108.80 K N5 O13 Zn3'
_cod_database_code               7059852
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.700
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              62167