New Routes to Transition Metal-Carbido Species: Synthesis and Characterization of the Carbon-Centered Trigonal Prismatic Clusters [W6CCl18]n- (n= 1, 2, 3)
Eric J. Welch; Nathan R. M. Crawford; Robert G. Bergman; Jeffrey R. Long; Journal of the American Chemical Society 125 (2003) 11464–11465; doi:10.1021/ja035962v

data_4114196
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 New Routes to Transition Metal-Carbido Species: Synthesis and
 Characterization of the Carbon-Centered Trigonal Prismatic Clusters
 [W6CCl18]n- (n= 1, 2, 3)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11464
_journal_page_last               11465
_journal_paper_doi               10.1021/ja035962v
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C79 H73 Cl18 N O P3 W6'
_chemical_formula_sum            'C79 H73 Cl18 N O P3 W6'
_chemical_formula_weight         2886.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 93.928(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.069(3)
_cell_length_b                   39.385(10)
_cell_length_c                   15.887(3)
_cell_measurement_reflns_used    5688
_cell_measurement_temperature    120
_cell_measurement_theta_max      49.25
_cell_measurement_theta_min      4.51
_cell_volume                     8782(3)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.0820
_diffrn_reflns_av_sigmaI/netI    0.1189
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37148
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    8.473
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             5428
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.692
_refine_diff_density_min         -3.012
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0.000001(0)
_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   0.989
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         14469
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_obs          0.0563
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1315
_refine_ls_wR_factor_obs         0.1117
_reflns_number_observed          9165
_reflns_number_total             14469
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035962vsi20030505_101753.cif
_cod_data_source_block           ejw14a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0567P)^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^)+(0.0567P)^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        8782.5(33)
_cod_database_code               4114196