Oxocyano complexes of molybdenum(IV) and tungsten(IV) with Schiff base ligands derived from salicylaldehyde and aliphatic amines. Crystal structure of [PPh4]2[Mo(CN)3O(ensal)]·5.5H2O (Hensal = N-salicylideneethylenediamine)
Nowicka, Beata; Samotus, Alina; Szklarzewicz, Janusz; Heinemann, Frank W.; Kisch, Horst; Journal of the Chemical Society, Dalton Transactions  (1998) 4009–; doi:10.1039/a805242e

data_7027000
_publ_section_title
;
 Oxocyano complexes of molybdenum(IV) and tungsten(IV) with Schiff base
 ligands derived from salicylaldehyde and aliphatic amines. Crystal
 structure of [PPh4]2[Mo(CN)3O(ensal)]&#x00B7;5.5H2O
 (Hensal&#x2005;=&#x2005;N-salicylideneethylenediamine)
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4009
_journal_paper_doi               10.1039/a805242e
_journal_year                    1998
_chemical_formula_sum            'C60 H62 Mo N5 O7.5 P2'
_chemical_formula_weight         1131.03
_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                69.38(2)
_cell_angle_beta                 73.90(4)
_cell_angle_gamma                82.67(3)
_cell_formula_units_Z            2
_cell_length_a                   12.384(5)
_cell_length_b                   14.309(3)
_cell_length_c                   17.745(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      11.00
_cell_measurement_theta_min      2.35
_cell_volume                     2826.0(16)
_computing_cell_refinement
'XSCAnS 2.10b (Siemens An. X-Ray Instr., 1994)'
_computing_data_collection
'XSCAnS 2.10b (Siemens An. X-Ray Instr., 1994)'
_computing_data_reduction
'XSCAnS 2.10b (Siemens An. X-Ray Instr., 1994)'
_computing_molecular_graphics
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_publication_material
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_refinement
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_solution
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from \w-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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.3562
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10644
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.08
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.346
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0041(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.884
_refine_ls_goodness_of_fit_obs   1.255
_refine_ls_hydrogen_treatment    'riding on preceding C or N atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         9450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_restrained_S_obs      1.255
_refine_ls_R_factor_all          0.2863
_refine_ls_R_factor_obs          0.0949
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2465
_refine_ls_wR_factor_obs         0.1880
_reflns_number_observed          2922
_reflns_number_total             9451
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            805242Esup1.cif
_cod_data_source_block           bb9702b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.0000P] 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^)+(0.0879P)^2^+0.0000P] 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        2826.0(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C60 H62 Mo N5 O7.50 P2'
_cod_database_code               7027000