Folded Cr12Co12 and Cr12Ni12 wheels: a sharp increase in nuclearity of heterometallic chromium rings
Christian Plenk; Thomas Weyhermuller; Eva Rentschler; Chem.Commun. 50 (2014) 3871–; doi:10.1039/C4CC00895B

data_7112177
_publ_section_title
;
 Folded Cr12Co12 and Cr12Ni12 wheels: a sharp increase in nuclearity of
 heterometallic chromium rings
;
_journal_name_full               Chem.Commun.
_journal_page_first              3871
_journal_paper_doi               10.1039/C4CC00895B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C272 H476 Co12 Cr12 N16 O112, 13(C3 H6 O)'
_chemical_formula_sum            'C311 H554 Co12 Cr12 N16 O125'
_chemical_formula_weight         7848.75
_chemical_name_systematic
;
octakis(\m3-hydroxo)-tetrakis(\m2-2,2'-bipyrimidine-N,N',N'',N''')
-octakis(\m2-hydroxo)-hexatriacontakis(\m2-pivalato)-tetrakis(pivalato-O,O')
-tetrakis(pivalato)-tetrakis(pivalic acid)-dodeca-chromium(III)
-dodeca-cobalt(II) tridecaacetone solvate 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 114.472(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.679(4)
_cell_length_b                   26.582(3)
_cell_length_c                   43.235(5)
_cell_measurement_reflns_used    9512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.4520
_cell_measurement_theta_min      2.1937
_cell_volume                     41505(8)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            1464879
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.910
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.91210
_exptl_absorpt_correction_T_min  0.72335
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       prism
_exptl_crystal_F_000             16576
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4583
_refine_ls_number_reflns         73103
_refine_ls_number_restraints     1481
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+482.1221P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                51850
_reflns_number_total             73103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00895b2.cif
_cod_data_source_block           cp207
_cod_database_code               7112177