W2Cl4(NR2)2(PR'3)2 Molecules. 7. Preparation, Characterization, and Structures of W2Cl4(NHR)2(NH2R)2 and W2Cl4(NHR)2(PMe3)2 (R =sec-Butyl and Cyclohexyl) and 31P{1H} NMR Studies of Trans-to-Cis Isomerizations of W2Cl4(NHR)2(PMe3)2
F. Albert Cotton; Evgeny V. Dikarev; Wai-Yeung Wong; Inorganic Chemistry 36 (1997) 3268–3276; doi:10.1021/ic961485o

data_4323502
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 7. Preparation, Characterization, and
 Structures of W2Cl4(NHR)2(NH2R)2 and W2Cl4(NHR)2(PMe3)2 (R =sec-Butyl and
 Cyclohexyl) and 31P{1H} NMR Studies of Trans-to-Cis Isomerizations of
 W2Cl4(NHR)2(PMe3)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3268
_journal_page_last               3276
_journal_paper_doi               10.1021/ic961485o
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C24 H50 Cl4 N4 W2'
_chemical_formula_structural     W2Cl4(NHCy)2(NH2Cy)2
_chemical_formula_sum            'C24 H50 Cl4 N4 W2'
_chemical_formula_weight         904.18
_chemical_melting_point          ?
_chemical_name_common
; 
 trans,trans-Tetrachloro-bis(cyclohexylamido)-bis(cyclohexylamine)
 ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(cyclohexylamido)-(trans,trans)-1,2-
 bis(cyclohexylamine) ditungsten(III) 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.782(2)
_cell_length_b                   12.782(2)
_cell_length_c                   9.943(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      14
_cell_volume                     1624.5(5)
_computing_cell_refinement       'TEXSAN-TEXRAY (1985)'
_computing_data_collection       'TEXSAN-TEXRAY (1985)'
_computing_data_reduction        'TEXSAN-TEXRAY (1985)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2742
_diffrn_reflns_theta_max         60.16
_diffrn_reflns_theta_min         4.89
_diffrn_standards_decay_%        11
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.060
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7970
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.357
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(8)
_refine_ls_extinction_coef       0.00038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1218
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_obs          0.0278
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+3.7742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0777
_refine_ls_wR_factor_obs         0.0657
_reflns_number_observed          779
_reflns_number_total             1219
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961485o_2.cif
_cod_data_source_block           W2Cl4(NHCy)2(NH2Cy)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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^)+(0.0236P)^2^+3.7742P] 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^)+(0.0236P)^2^+3.7742P] 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               4323502