Co-assembly of a three-dimensional open framework sulfide with a novel linkage between an oxygen-encapsulated T3 cluster and a supertetrahedral T2 cluster
Xiaohui Han; Zhenqing Wang; Dan Liu; Jin Xu; Yongxin Liu; Cheng Wang; Chem.Commun. 50 (2014) 796–; doi:10.1039/c3cc45439h

data_7110245
_publ_section_title
;
 Co-assembly of a three-dimensional open framework sulfide with a novel
 linkage between an oxygen-encapsulated T3 cluster and a supertetrahedral
 T2 cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              796
_journal_paper_doi               10.1039/c3cc45439h
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C10.8 H25.2 Ga0.8 N1.8 O2.8 S6.5 Sn2.7'
_chemical_formula_weight         809.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           112
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2c'
_symmetry_space_group_name_H-M   'P -4 2 c'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.6663(3)
_cell_length_b                   14.6663(3)
_cell_length_c                   24.9609(11)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.55
_cell_volume                     5369.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26534
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    3.800
_exptl_absorpt_correction_T_max  0.7768
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             3110
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
A large region of solvent molecules in the lattice could not be modelled from 
F-maps as high degree of statistical and positional disorder. 
We employed PLATON SQUEEZE to calculate the contribution to the diffraction 
from the solvent region and thereby produced a set of solvent-free diffraction 
intensities. SQUEEZE estimated a total count of 3154 electrons per unit cell, 
which were assigned to be 14.4 H+-DMMP molecules per unit cell.
The final formula was calculated from TGA combined with elemental analysis data.
;
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         4739
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0954P)^2^+4.1712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                3805
_reflns_number_total             4739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45439h.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-42c
_cod_original_formula_sum
'C10.80 H25.20 Ga0.80 N1.80 O2.80 S6.50 Sn2.70'
_cod_database_code               7110245