Proton NMR Study of Cr-Co Heterometallic Wheel Complexes
E. Carolina Sañudo; Thomas B. Faust; Christopher A. Muryn; Robin G. Pritchard; Grigore A. Timco; Richard E. P. Winpenny; Inorganic Chemistry 48 (2009) 9811–9818; doi:10.1021/ic901418z

data_4303416
_publ_section_title
;
Proton NMR Study of Cr-Co Heterometallic Wheel Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9811
_journal_page_last               9818
_journal_paper_doi               10.1021/ic901418z
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C86 H156 Co1 Cr7 F8 N2 Na1 O33 S1'
_chemical_formula_sum            'C86 H156 Co Cr7 F8 N2 Na O33 S'
_chemical_formula_weight         2376.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-03-25T00:28:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.4145(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6702(3)
_cell_length_b                   25.7942(4)
_cell_length_c                   26.3871(4)
_cell_measurement_reflns_used    18807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     13376.3(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.384752E-1
_diffrn_orient_matrix_UB_12      0.84017E-2
_diffrn_orient_matrix_UB_13      -0.246092E-1
_diffrn_orient_matrix_UB_21      -0.286315E-1
_diffrn_orient_matrix_UB_22      -0.270239E-1
_diffrn_orient_matrix_UB_23      0.159424E-1
_diffrn_orient_matrix_UB_31      -0.170009E-1
_diffrn_orient_matrix_UB_32      0.264974E-1
_diffrn_orient_matrix_UB_33      0.240621E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            144841
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        22
_diffrn_reflns_theta_max         22
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.061
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.18
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1255
_refine_ls_number_reflns         16346
_refine_ls_number_restraints     1716
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+53.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2302
_reflns_number_gt                9057
_reflns_number_total             16346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901418z_si_001_6.cif
_cod_data_source_block           shelxl_NaDMSOMeCNCr7Co-8B
_cod_database_code               4303416