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_4322299
_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(O)(S2)2(SPh)]'
_chemical_formula_sum            'C54 H45 Nb O P2 S5'
_chemical_formula_weight         1025.05
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                103.580(10)
_cell_angle_beta                 95.550(10)
_cell_angle_gamma                101.420(10)
_cell_formula_units_Z            2
_cell_length_a                   10.853(2)
_cell_length_b                   10.9760(10)
_cell_length_c                   21.641(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2428.3(6)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4541
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0.9
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.568
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+3.8006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1001
_refine_ls_wR_factor_obs         0.0964
_reflns_number_observed          3945
_reflns_number_total             4541
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981328k_1.cif
_cod_data_source_block           '[(C6H5)4P]2[Nb(O)(S2)2(SPh)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'triclic' was replaced with
'triclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+3.8006P] 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^)+(0.0374P)^2^+3.8006P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322299