Structure and bonding in the d4/d3 alkyne redox pairs [WX(CO)(MeCCMe)Tp′]z (X = F, Cl, Br and I; z = 0 and 1): halide stabilisation of electron deficient metal alkyne complexes
Bartlett, Ian M.; Carlton, Susannah; Connelly, Neil G.; Harding, David J.; Hayward, Owen D.; Guy Orpen, A.; Ray, Christopher D.; Rieger, Philip H.; Chemical Communications  (1999) 2403–; doi:10.1039/a907912b

data_7110735
_publ_section_title
;
 Structure and bonding in the d4/d3 alkyne redox pairs
 [WX(CO)(MeC&#xE007;CMe)Tp&#x2032;]z (X = F, Cl, Br and I; z = 0 and 1):
 halide stabilisation of electron deficient metal alkyne complexes
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2403
_journal_paper_doi               10.1039/a907912b
_journal_year                    1999
_chemical_formula_sum            'C25.5 H29 B Br Cl3 N6 O W'
_chemical_formula_weight         816.47
_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                88.34(1)
_cell_angle_beta                 70.03(2)
_cell_angle_gamma                78.05(1)
_cell_formula_units_Z            2
_cell_length_a                   10.297(3)
_cell_length_b                   11.663(2)
_cell_length_c                   13.935(2)
_cell_measurement_reflns_used    164
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      1.79
_cell_volume                     1537.2(6)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12294
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    5.348
_exptl_absorpt_correction_T_max  0.677153
_exptl_absorpt_correction_T_min  0.419749
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick 1996'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.868
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                4104
_reflns_number_total             4832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907912bsup1.cif
_cod_data_source_block           '[WBr(CO)(MeCCMe)Tp']'
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1537.2(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C25.50 H29 B Br Cl3 N6 O W'
_cod_database_code               7110735