A Chelate-Stabilized Tungsten‒Imido‒Monoalkyl Complex, [WCl(PhN)(CH~2~CMe~3~){<i>o</i>-C~6~H~4~(NSiMe~3~)~2~}]
Wang, S.-Y. S.; Boncella, J. M.; Abboud, K. A.; Acta Crystallographica Section C 53 (1997) 436–438; doi:10.1107/S0108270196014370

data_2006031
_publ_section_title
;
 A Chelate-Stabilized Tungsten--Imido--Monoalkyl Complex,
 [WCl(PhN)(CH~2~CMe~3~){<i>o</i>-C~6~H~4~(NSiMe~3~)~2~}]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              436
_journal_page_last               438
_journal_paper_doi               10.1107/S0108270196014370
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C23 H38 Cl N3 Si2 W'
_chemical_formula_weight         632.04
_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'
_audit_creation_method           SHELXTL
_cell_angle_alpha                96.705(1)
_cell_angle_beta                 93.814(1)
_cell_angle_gamma                111.296(1)
_cell_formula_units_Z            2
_cell_length_a                   9.3531(1)
_cell_length_b                   11.2640(2)
_cell_length_c                   14.1166(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     1366.63(4)
_computing_cell_refinement       'SMART and SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SHELXTL95 (Sheldrick, 1995)'
_computing_molecular_graphics    SHELXTL95
_computing_publication_material  SHELXTL95
_computing_structure_refinement  SHELXTL95
_computing_structure_solution    SHELXTL95
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'SMART PLATFORM'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8884
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        <1
_diffrn_standards_number         'see text'
_exptl_absorpt_coefficient_mu    4.43
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   'integration (SHELXTL95; Sheldrick, 1995)'
_exptl_crystal_colour            'Red  '
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.46
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_method     SHELXTL95
_refine_ls_goodness_of_fit_all   1.08
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_obs          0.034
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0448P)^2^+3.7698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.091
_refine_ls_wR_factor_obs         0.0850
_reflns_number_observed          5743
_reflns_number_total             6107
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1269.cif
_cod_data_source_block           I
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0448P)^2^+3.7698P] 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^)+(0.0448P)^2^+3.7698P] 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        1366.63(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2006031