[PPh4]3[W(CN)7(O2)]·4H2O as the Representative of the [M(L)7(LL)] Class for Nine-Coordinate Complexes
Matoga, Dariusz; Szklarzewicz, Janusz; Mikuriya, Masahiro; Inorganic Chemistry 45 (2006) 7100–7104; doi:10.1021/ic060523t

data_4332560
_publ_section_title
;
 [PPh4]3[W(CN)7(O2)]&#x00B7;4H2O as the Representative of the [M(L)7(LL)]
 Class for Nine-Coordinate Complexes
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7100
_journal_page_last               7104
_journal_paper_doi               10.1021/ic060523t
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C79 H68 N7 O6 P3 W'
_chemical_formula_weight         1488.15
_chemical_name_systematic
; 
 (PPh4)3[W(CN)7(O2)]4H2O 
;
_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                77.8710(10)
_cell_angle_beta                 87.181(2)
_cell_angle_gamma                62.9770(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1951(11)
_cell_length_b                   13.9814(12)
_cell_length_c                   21.5885(18)
_cell_measurement_temperature    291(2)
_cell_volume                     3463.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'psi 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  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21526
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.8000
_exptl_absorpt_correction_T_min  0.4222
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.494
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         15266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0467P)^2^+1.2998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                12816
_reflns_number_total             15266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060523tsup1.cif
_cod_data_source_block           wcn71
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332560