Monomeric Niobium Persulfide Complexes: The Synthesis and Structural Characterization of Pentagonal-Pyramidal [Ph4P]2[Nb(E)(S2)2(SPh)] (E = O, S) Complexes
Jung Woo Park; Sang Man Koo; Inorganic Chemistry 38 (1999) 4898–4900; doi:10.1021/ic981328k

data_4322300
_publ_section_title
;
 Monomeric Niobium Persulfide Complexes: The Synthesis and Structural
 Characterization of Pentagonal-Pyramidal [Ph4P]2[Nb(E)(S2)2(SPh)] (E = O,
 S) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4898
_journal_page_last               4900
_journal_paper_doi               10.1021/ic981328k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     '[(C6H5)4P]2[Nb(S)(S2)2(SPh)]'
_chemical_formula_sum            'C54 H45 Nb P2 S6'
_chemical_formula_weight         1041.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.821(5)
_cell_length_b                   21.559(8)
_cell_length_c                   21.273(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4949(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.1094
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5262
_diffrn_reflns_theta_max         20.02
_diffrn_reflns_theta_min         1.89
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.597
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.156
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.156
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         0.807
_refine_ls_shift/esd_mean        0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+10.4466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1760
_refine_ls_wR_factor_obs         0.1350
_reflns_number_observed          2554
_reflns_number_total             4579
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981328k_2.cif
_cod_data_source_block           '[(C6H5)4P]2[Nb(S)(S2)2(SPh)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+10.4466P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+10.4466P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4949.3(34)
_cod_database_code               4322300