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_7112178
_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 Cr12 N16 Ni12 O112, 9(C3 H6 O)'
_chemical_formula_sum            'C299 H530 Cr12 N16 Ni12 O121'
_chemical_formula_weight         7613.88
_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-nickel(II) nonaacetone 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                 113.9190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.8265(9)
_cell_length_b                   26.8781(7)
_cell_length_c                   43.4526(10)
_cell_measurement_reflns_used    102141
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      0.90
_cell_volume                     42519.6(18)
_computing_cell_refinement       'APEX2 V2.0(Bruker, 2006)'
_computing_data_collection       'APEX2 V2.0(Bruker, 2006)'
_computing_data_reduction        'APEX2 V2.0(Bruker, 2006)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       '\k-geometry diffractometry'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2683
_diffrn_reflns_av_unetI/netI     0.1554
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            744307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.970
_diffrn_reflns_theta_min         0.899
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.7593
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Platon; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             16112
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.330
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4543
_refine_ls_number_reflns         102141
_refine_ls_number_restraints     2402
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.2212
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+104.8663P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.3040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43268
_reflns_number_total             102141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00895b2.cif
_cod_data_source_block           cp208
_cod_database_code               7112178