Syntheses, Structures, and Nonlinear Optical Properties of Heteroselenometallic W−Se−Ag Cluster Compounds Containing Phosphine Ligands
Zhang, Qian-Feng; Ding, Jihai; Yu, Zhan; Song, Yinglin; Rothenberger, Alexander; Fenske, Dieter; Leung, Wa-Hung; Inorganic Chemistry 45 (2006) 8638–8647; doi:10.1021/ic0610839

data_4332916
_publ_section_title
;
 Syntheses, Structures, and Nonlinear Optical Properties of
 Heteroselenometallic W&#x2212;Se&#x2212;Ag Cluster Compounds Containing
 Phosphine Ligands
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8638
_journal_page_last               8647
_journal_paper_doi               10.1021/ic0610839
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C54 H99 Ag3 I P3 Se4 W'
_chemical_formula_weight         1791.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   37.2352(5)
_cell_length_b                   11.70240(10)
_cell_length_c                   14.9951(2)
_cell_measurement_reflns_used    9034
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.19
_cell_volume                     6533.98(14)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79693
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    5.446
_exptl_absorpt_correction_T_max  0.6201
_exptl_absorpt_correction_T_min  0.3169
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13601
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0131P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                10256
_reflns_number_total             13601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0610839sup1.cif
_cod_data_source_block           '[(WSe4)Ag3(PCy3)3I]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4332916