Synthesis, structure and magnetic properties of a novel high-nuclearity oxo-carboxylate [Zn<sub>x</sub>Co<sub>13-x</sub>(μ<sub>4</sub>-O)<sub>4</sub>(O<sub>2</sub>CPh)<sub>18</sub>] cluster.
Nawrocki, Jan; Prochowicz, Daniel; Justyniak, Iwona; van Leusen, Jan; Kornowicz, Arkadiusz; Kögerler, Paul; Lewiński, Janusz; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12828–12831; doi:10.1039/c9dt02791b

data_7700768
_publ_section_title
;
 Synthesis, structure and magnetic properties of a novel high-nuclearity
 oxo-carboxylate
 [Zn<sub>x</sub>Co<sub>13-x</sub>(\m<sub>4</sub>-O)<sub>4</sub>(O<sub>2</sub>CPh)<sub>18</sub>]
 cluster.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12828
_journal_page_last               12831
_journal_paper_doi               10.1039/c9dt02791b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C126 H90 Co6 O40 Zn7'
_chemical_formula_weight         3055.14
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-05-21 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.1339(5)
_cell_length_b                   22.1339(5)
_cell_length_c                   26.6450(6)
_cell_measurement_reflns_used    11796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7992
_cell_measurement_theta_min      3.1818
_cell_volume                     11304.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details
;
  1 omega  -48.00   -2.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764  -57.0000  -90.0000 46

  2 omega   -8.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764  -99.0000  -30.0000 30

  3 omega  -81.00  -42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764  -57.0000    0.0000 39

  4 omega  -33.00   40.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764   37.0000  -60.0000 73

  5 omega  -91.00  -64.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764  -57.0000  120.0000 27

  6 omega  -46.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1764  -57.0000 -180.0000 49

  7 omega   68.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7545   57.0000 -180.0000 25

  8 omega  -46.00   46.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7545  -57.0000   30.0000 92

  9 omega   -7.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7545   77.0000  150.0000 100

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10951
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.863
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       cubic
_exptl_crystal_F_000             4614
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         10951
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0944P)^2^+6.8494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                8939
_reflns_number_total             10951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02791b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7700768.cif.'
_cod_original_cell_volume        11304.8(6)
_cod_database_code               7700768
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              35665