Zinc(II) and Cadmium(II) Monohydroxide Bridged, Dinuclear Metallacycles: A Unique Case of Concerted Double Berry Pseudorotation
Daniel L. Reger; Andrea E. Pascui; Perry J. Pellechia; Mark D. Smith; Inorganic Chemistry 52 (2013) 11638–11649; doi:10.1021/ic402073d

data_4336382
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       reger@mailbox.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Daniel L. Reger'
_publ_contact_author_phone       '1 803 777 2587'
_publ_section_title
;
 Zinc(II) and Cadmium(II) Monohydroxide Bridged, Dinuclear Metallacycles:
 A Unique Case of Concerted Double Berry Pseudorotation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11638
_journal_page_last               11649
_journal_paper_doi               10.1021/ic402073d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C40 H37 N16 O Zn2, 1.5(C2 H3 N), 3(Cl O4)'
_chemical_formula_sum            'C43 H41.5 Cl3 N17.5 O13 Zn2'
_chemical_formula_weight         1248.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.797(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3497(9)
_cell_length_b                   42.817(4)
_cell_length_c                   11.9166(9)
_cell_measurement_reflns_used    2659
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.818
_cell_measurement_theta_min      2.224
_cell_volume                     5169.2(8)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.1046
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27354
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       bar
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1706
_reflns_number_gt                4410
_reflns_number_total             8069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402073d_si_002_3.cif
_cod_data_source_block           1_1.5CH3CN
_cod_original_cell_volume        5169.2(7)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C43 H41.50 Cl3 N17.50 O13 Zn2'
_cod_database_code               4336382