W2Cl4(NR2)2(PR'3)2 Molecules. 5. Preparation and Characterization of W2Cl4(NEt2)2(L-L) (L-L = dmpm, dmpe, dppe), W2Cl4(NBu2)2(L-L) (L-L = dmpm, dmpe), and W2Cl4(NHex2)2(dmpm). First Complexes with Bridging Diphosphine Ligands in a cis,trans-Stereochemistry
F. Albert Cotton; Evgeny V. Dikarev; Wai-Yeung Wong; Inorganic Chemistry 36 (1997) 902–912; doi:10.1021/ic961151z

data_4323336
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 5. Preparation and Characterization of
 W2Cl4(NEt2)2(L-L) (L-L = dmpm, dmpe, dppe), W2Cl4(NBu2)2(L-L) (L-L =
 dmpm, dmpe), and W2Cl4(NHex2)2(dmpm). First Complexes with Bridging
 Diphosphine Ligands in a cis,trans-Stereochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              902
_journal_page_last               912
_journal_paper_doi               10.1021/ic961151z
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C15 H38 C16 N2 P2 W2'
_chemical_formula_structural     cis,trans-W2Cl4(Et2N)2(DMPE).CH2Cl2
_chemical_formula_sum            'C15 H38 Cl6 N2 P2 W2'
_chemical_formula_weight         888.81
_chemical_name_common
;
 cis,trans-Tetrachloro-bis(diethylamido)-dimethyl-
 phosphinoethan ditungsten(III)
;
_chemical_name_systematic
;
 1,1,2,2-Tetrachloro-1,2-bis(diethylamido)-(cis,trans)-
 1,2-dimethylphosphinoethan ditungsten(III)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.73(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.596(2)
_cell_length_b                   15.975(2)
_cell_length_c                   18.756(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      18.0
_cell_volume                     2855.4(9)
_computing_cell_refinement       'CAD4 V.5.0'
_computing_data_collection       'CAD4 V.5.0'
_computing_data_reduction        'SDP (Enraf-Nonius, 1979)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6560
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.731
_exptl_absorpt_correction_T_max  0.9993
_exptl_absorpt_correction_T_min  0.5537
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.152
_refine_ls_goodness_of_fit_obs   1.170
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_restrained_S_obs      1.170
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_obs          0.0257
_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^)+(0.0321P)^2^+5.9807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0706
_refine_ls_wR_factor_obs         0.0653
_reflns_number_observed          5620
_reflns_number_total             6190
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961151z_8.cif
_cod_data_source_block           W2Cl4(NEt2)2(DMPE).CH2Cl2
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+5.9807P] 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^)+(0.0321P)^2^+5.9807P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323336