Synthesis, crystal structure and properties of sandwich type compounds based on {AsW9} and a hexa-nuclear unit with three supporting TM‒triazole complexes
Liu, Jia-min; Wang, Lu; Yu, Kai; Su, Zhan-hua; Wang, Chun-xiao; Wang, Chun-mei; Zhou, Bai-bin; New J. Chem. 39 (2015) 1139–; doi:10.1039/C4NJ01138D

data_7054462
_publ_section_title
;
 Synthesis, crystal structure and properties of sandwich type compounds
 based on {AsW9} and a hexa-nuclear unit with three supporting
 TM--triazole complexes
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1139
_journal_paper_doi               10.1039/C4NJ01138D
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C6 H34 As2 Co3 N9 Na9 O77 W18'
_chemical_formula_sum            'C6 H34 As2 Co3 N9 Na9 O77 W18'
_chemical_formula_weight         5307.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   13.9307(5)
_cell_length_b                   13.9307(5)
_cell_length_c                   33.554(3)
_cell_measurement_reflns_used    8571
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.43
_cell_volume                     5639.2(6)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            40515
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    19.403
_exptl_absorpt_correction_T_max  0.0697
_exptl_absorpt_correction_T_min  0.0543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.128
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4649.0
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_platon_squeeze_details          ' ? '
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0550P)^2^+245.7718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                3650
_reflns_number_total             4805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01138d2.cif
_cod_data_source_block           ljm001410_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7054460--7054462.cif.
;
_cod_original_cell_volume        5639.2(5)
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7054462