Formation of a Tetranuclear Copper (II) Cluster Assembled by Metal-Assisted Hydrolysis and Desulfurization of Bis(3,5-dimethylpyrazolyl)methylphosphine Sulfide, MeP(S)(3,5-Me2Pz)2#
V. Chandrasekhar; S. Kingsley; A. Vij; K. C. Lam; A. L. Rheingold; Inorganic Chemistry 39 (2000) 3238–3242; doi:10.1021/ic991255k

data_4321182
_publ_contact_author
; 
     Chandrasekhar. V.
     Department of Chemistry
     IIT, Kanpur 208 016
     India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 435'
_publ_section_title
;
 Formation of a Tetranuclear Copper (II) Cluster Assembled by
 Metal-Assisted Hydrolysis and Desulfurization of
 Bis(3,5-dimethylpyrazolyl)methylphosphine Sulfide, MeP(S)(3,5-Me2Pz)2#
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3238
_journal_page_last               3242
_journal_paper_doi               10.1021/ic991255k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C11 H17 N4 P S'
_chemical_formula_weight         268.33
_chemical_melting_point          70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 93.349(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2552(1)
_cell_length_b                   8.7364(2)
_cell_length_c                   21.4490(3)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2853.74(8)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, Ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD'
_diffrn_measurement_method       '\w oscillation, 0.3 deg'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7879
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 'beginning & end'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.9477
_exptl_absorpt_correction_T_min  0.8708
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0010
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+2.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                2440
_reflns_number_total             2876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991255k_2.cif
_cod_data_source_block           for-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4321182