A monovacant heteropolytungstate-incorporated trimeric carbonyl rhenium cluster, [(AsW11O39){Re(CO)3}3(μ3-OH)(μ2-OH)]6−: synthesis, structure and catalytic properties
Zhang, Yanhui; Zhang, Dongdi; Huo, Zhiyuan; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; RSC Advances 4 (2014) 28848–; doi:10.1039/c4ra03532a

data_7217022
_publ_section_title
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 A monovacant heteropolytungstate-incorporated trimeric carbonyl rhenium
 cluster, [(AsW11O39){Re(CO)3}3(\m3-OH)(\m2-OH)]6&#x2212;: synthesis,
 structure and catalytic properties
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_journal_issue                   55
_journal_name_full               'RSC Advances'
_journal_page_first              28848
_journal_paper_doi               10.1039/c4ra03532a
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C88 H207 As4 N13 O216 Re12 W44'
_chemical_formula_weight         15527.15
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.4276(4)
_cell_length_b                   23.4276(4)
_cell_length_c                   32.0967(9)
_cell_measurement_reflns_used    6872
_cell_measurement_temperature    124.8(3)
_cell_measurement_theta_max      29.1956
_cell_measurement_theta_min      3.0224
_cell_volume                     17616.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      124.8(3)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.1161
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37079
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    18.856
_exptl_absorpt_correction_T_max  0.1240
_exptl_absorpt_correction_T_min  0.0454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13684
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.334
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         13383
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0599P)^2^+25.1349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                9291
_reflns_number_total             13383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra03532a2.cif
_cod_data_source_block           p121223a1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-421c
_cod_database_code               7217022