Ti2-Containing 18-Tungsto-2-Arsenate(III) Monolacunary Host and the Incorporation of a Phenylantimony(III) Guest.
Wang, Kai-Yao; Lin, Zhengguo; Bassil, Bassem S.; Xing, Xiaolin; Haider, Ali; Keita, Bineta; Zhang, Guangjin; Silvestru, Cristian; Kortz, Ulrich; Inorganic chemistry 54 (2015) 10530–10532; doi:10.1021/acs.inorgchem.5b01863

data_4346641
_publ_section_title
;
 Ti2-Containing 18-Tungsto-2-Arsenate(III) Monolacunary Host and the
 Incorporation of a Phenylantimony(III) Guest.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10530
_journal_page_last               10532
_journal_paper_doi               10.1021/acs.inorgchem.5b01863
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C6 H85 As2 Cs2.5 Na9.5 O108 Sb Ti2 W18'
_chemical_formula_weight         6113.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 91.7750(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7957(4)
_cell_length_b                   27.7898(7)
_cell_length_c                   19.7359(5)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.54
_cell_volume                     10303.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            200507
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         3.428
_exptl_absorpt_coefficient_mu    22.080
_exptl_absorpt_correction_T_max  0.271
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.941
_exptl_crystal_description       block
_exptl_crystal_F_000             10880
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.271
_exptl_transmission_factor_min   0.177
_refine_diff_density_max         4.320
_refine_diff_density_min         -4.444
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         24537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+320.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19210
_reflns_number_total             24537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01863_si_002.cif
_cod_data_source_block           wky
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C6 H85 As2 Cs2.50 Na9.50 O108 Sb Ti2 W18'
_cod_database_code               4346641
_shelx_estimated_absorpt_t_min   0.177
_shelx_estimated_absorpt_t_max   0.271
_shelxl_version_number           2014-3
_shelx_res_checksum              69764
_shelx_hkl_checksum              30463