Synthesis and structure of a series of tungsten(ii) and tungsten(vi) diynyl and diyndiyl complexes
Roberts, Rachel L.; Puschmann, Horst; Howard, Judith A. K.; Yamamoto, John H.; Carty, Arthur J.; Low, Paul J.; Dalton Transactions  (2003) 1099–; doi:10.1039/b212074g

data_7012550
_publ_section_title
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 Synthesis and structure of a series of tungsten(ii) and tungsten(vi)
 diynyl and diyndiyl complexes
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1099
_journal_paper_doi               10.1039/b212074g
_journal_year                    2003
_chemical_formula_moiety         'C24 H30 O4 W2'
_chemical_formula_sum            'C24 H30 O4 W2'
_chemical_formula_weight         750.18
_chemical_name_common
;
bis((1,2,3,4,5-pentamethyl cyclopentadienyl)(dioxo)tungsten)
buta-1,3-diyn-1,4-diyl
;
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6091(5)
_cell_length_b                   12.1041(4)
_cell_length_c                   15.4689(6)
_cell_measurement_reflns_used    6342
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.993
_cell_measurement_theta_min      2.634
_cell_volume                     2360.89(15)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD 6K area detector'
_diffrn_measurement_method       \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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16192
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    9.763
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            light_yellow
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.732
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0192P)^2^+5.9062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                2872
_reflns_number_total             3396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212074g.txt
_cod_data_source_block           02srv044Compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured'' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7012550