Bis(3,5-dimethylpyrazol-1-yl)acyl and Bis(3,5-dimethylpyrazol-1-yl)methide Carbonyl Tungsten Derivatives
Xie, Yun-Fu; Wen, Zhen-Kang; Tan, Run-Yu; Hong, Juan; Zhao, Shu-Bin; Tang, Liang-Fu; Organometallics 27 (2008) 5684–; doi:10.1021/om800603p

data_4072131
_publ_section_title
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 Bis(3,5-dimethylpyrazol-1-yl)acyl and
 Bis(3,5-dimethylpyrazol-1-yl)methide Carbonyl Tungsten Derivatives
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_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5684
_journal_paper_doi               10.1021/om800603p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C14 H15 Cl N4 O3 W'
_chemical_formula_weight         506.60
_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-97
_cell_angle_alpha                81.941(5)
_cell_angle_beta                 81.338(4)
_cell_angle_gamma                73.698(4)
_cell_formula_units_Z            4
_cell_length_a                   9.196(2)
_cell_length_b                   14.033(3)
_cell_length_c                   14.305(3)
_cell_measurement_reflns_used    1219
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      19.12
_cell_measurement_theta_min      2.32
_cell_volume                     1742.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi 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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.2067
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9929
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    6.801
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.625998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                3162
_reflns_number_total             7025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800603p_si_001.cif
_cod_data_source_block           figure4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1742.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072131