Zinc Chalcogenolate Complexes as Precursors to ZnE and Mn/ZnE (E = S, Se) Clusters
Chhatra B. Khadka; Andreas Eichhöfer; Florian Weigend; John F. Corrigan; Inorganic Chemistry 51 (2012) 2747–2756; doi:10.1021/ic200307g

data_4328475
_publ_contact_author_address
;Dept of Chemistry
The University of Western Ontario
London ON
N6A 5B7
;
_publ_contact_author_email       corrigan@uwo.ca
_publ_contact_author_name        'J. Corrigan'
_publ_section_title
;
 Zinc Chalcogenolate Complexes as Precursors to ZnE and Mn/ZnE (E = S, Se)
 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2747
_journal_page_last               2756
_journal_paper_doi               10.1021/ic200307g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C39.5 H103 Cl9 Mn5.6 N12 Se13 Zn8.4'
_chemical_formula_weight         2948.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   25.5250(3)
_cell_length_b                   25.5250(3)
_cell_length_c                   27.9532(5)
_cell_measurement_reflns_used    39451
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.04
_cell_volume                     15772.3(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1303
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32468
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    7.282
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             8211
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         18498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+7.4193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                11601
_reflns_number_total             18498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200307g_si_002_4.cif
_cod_data_source_block           2d
_cod_original_cell_volume        15772.2(4)
_cod_original_sg_symbol_Hall     'P 31 2" '
_cod_original_formula_sum        'C39.50 H103 Cl9 Mn5.60 N12 Se13 Zn8.40'
_cod_database_code               4328475