Uncorrelated Dynamical Processes in Tetranuclear Carboxylate Clusters Studied by Variable-Temperature 1H NMR Spectroscopy.
Femke F. B. J. Janssen; Laurens C. J. M. Peters; Paul P. J. Schlebos; Jan M. M. Smits; René de Gelder; Alan E. Rowan; Inorganic Chemistry 52 (2013) 13004–13013; doi:10.1021/ic401522v

data_4336706
_publ_contact_author
;
        F.F.B.J. Janssen
        Institute for Molecules and Materials
        Radboud University Nijmegen
        Heyendaalseweg 135
        6525 AJ  Nijmegen
        The Netherlands
;
_publ_contact_author_email       femke.janssen@science.ru.nl
_publ_contact_author_fax         '031 024 3553450'
_publ_contact_author_phone       '031 024 3652022'
_publ_section_title
;
 Uncorrelated Dynamical Processes in Tetranuclear Carboxylate Clusters
 Studied by Variable-Temperature 1H NMR Spectroscopy.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13004
_journal_page_last               13013
_journal_paper_doi               10.1021/ic401522v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C71 H58 N6 O14 Zn4'
_chemical_formula_weight         1480.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-07-27
_audit_creation_method           'SHELXL, adapted and expanded'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3210(17)
_cell_length_b                   15.815(2)
_cell_length_c                   25.080(3)
_cell_measurement_reflns_used    153
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.010
_cell_volume                     6467.1(13)
_computing_data_collection
;
Nonius "Collect" program suite (Nonius, 1999)
;
_computing_data_reduction
;
Nonius "EvalCCD" program suite (Duisenberg, 1998)
;
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF (Beurskens et al., 1996),
PATTY (Beurskens et al., 1987)
;
_diffrn_ambient_temperature      208(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'area detector \f and \w scan'
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            96004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0.000
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS multi-scan (Sheldrick, 1996)'
_exptl_crystal_colour            'translucent light brown / orange'
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       'rather regular fragment'
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         14604
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0648
_refine_ls_R_factor_obs          0.0648
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+12.1799P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1566
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_obs         0.1351
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                8722
_reflns_number_observed          8722
_reflns_number_total             14604
_reflns_observed_criterion       >2sigma(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401522v_si_001_4.cif
_cod_data_source_block           FEMK80
_cod_original_cell_volume        6467.0(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336706