Novel hepta-coordinated molybdenum(ii) and tungsten(ii) carbene complexes by oxidative decarbonylation of Mo(0) and W(0) carbene complexes
Jaeger, Monika; Stumpf, Rüdiger; Troll, Carsten; Fischer, Helmut; Chemical Communications  (2000) 931–; doi:10.1039/b002228o

data_7110935
_publ_section_title
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 Novel hepta-coordinated molybdenum(ii) and tungsten(ii) carbene complexes
 by oxidative decarbonylation of Mo(0) and W(0) carbene complexes
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              931
_journal_paper_doi               10.1039/b002228o
_journal_year                    2000
_chemical_formula_moiety         'C13 H12 Cl4 O5 W'
_chemical_formula_sum            'C13 H12 Cl4 O5 W'
_chemical_formula_weight         573.9
_chemical_name_systematic
;                                                                           
Tricarbonyl(dicloro){O,C-[methoxy(o-methoxyphenyl)carbene]}tungsten          
;
_chemical_temperature_decomposition 80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_date             10-03-00
_audit_creation_method           'CIFEX (AG Fischer, 1994)'
_cell_angle_alpha                90
_cell_angle_beta                 100.57(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.567(6)
_cell_length_b                   11.994(6)
_cell_length_c                   15.986(5)
_cell_volume                     1803.2(16)
_computing_data_collection       'Siemens P3/V software 1989'
_computing_structure_refinement  'Siemens SHELXTL PLUS (VMS) 1990'
_computing_structure_solution    'Siemens SHELXTL PLUS (VMS) 1990'
_diffrn_ambient_temperature      300
_diffrn_measurement_device       'Siemens R3m/V diffractometer'
_diffrn_measurement_method       wyckoff
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4391
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.160
_exptl_absorpt_correction_T_max  0.1963
_exptl_absorpt_correction_T_min  0.1318
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.089
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_hydrogen_treatment    'riding with fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_obs          0.034
_refine_ls_shift/esd_max         0.0008
_refine_ls_shift/esd_mean        0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w=1/(\s^2^(F) + 0.00030 F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.041
_refine_ls_wR_factor_obs         0.037
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_observed          2782
_reflns_number_total             3949
_reflns_observed_criterion       'reflns observed if F > 4.0 \s(F)'
_cod_data_source_file            b002228osup1.cif
_cod_data_source_block           RSC
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '80
(decomp)'. The value '80 (decomp)' was changed to '80'.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/(\s^2^(F) + 0.00030
F^2^)' 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^(F) +
0.00030 F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1803.3(15)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7110935