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_4336380
_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         'C56 H69 Cd2 N16 O, 4(C2 H3 N), 3(Cl O4)'
_chemical_formula_sum            'C64 H81 Cd2 Cl3 N20 O13'
_chemical_formula_weight         1669.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.5580(10)
_cell_angle_beta                 70.0970(10)
_cell_angle_gamma                85.4280(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8807(5)
_cell_length_b                   13.4098(6)
_cell_length_c                   13.9681(7)
_cell_measurement_reflns_used    8505
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.782
_cell_measurement_theta_min      2.404
_cell_volume                     1878.08(15)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31071
_diffrn_reflns_theta_full        27.79
_diffrn_reflns_theta_max         27.79
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       rod
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8856
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0531P)^2^+1.4291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                8090
_reflns_number_total             8856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402073d_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4336380