The rational synthesis of (10,3)-type MOFs based on tetranuclear [W(Mo)OS3Cu3]+ secondary building units
Yao, Xiao-Qiang; Pan, Zhao-Rui; Hu, Jin-Song; Li, Yi-Zhi; Guo, Zi-Jian; Zheng, He-Gen; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 10049–10051; doi:10.1039/c1cc12691a

data_7106808
_publ_section_title
;
 The rational synthesis of (10,3)-type MOFs based on tetranuclear [W(Mo)OS3Cu3]+
 secondary building units
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   36
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              10049
_journal_page_last               10051
_journal_paper_doi               10.1039/c1cc12691a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C45 H35 Cu3 Mo N10 O S3, I'
_chemical_formula_sum            'C45 H35 Cu3 I Mo N10 O S3'
_chemical_formula_weight         1241.47
_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                74.739(6)
_cell_angle_beta                 76.360(5)
_cell_angle_gamma                80.407(5)
_cell_formula_units_Z            2
_cell_length_a                   12.004(5)
_cell_length_b                   12.215(5)
_cell_length_c                   16.157(7)
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.37
_cell_measurement_theta_min      2.61
_cell_volume                     2207.2(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11934
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.595
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                5934
_reflns_number_total             8459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12691a.txt
_cod_data_source_block           cluster1
_cod_original_cell_volume        2207.1(16)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7106808