Mixed Chloride/Amine Complexes of Dimolybdenum(II). 1. Preparation, Characterization, and Crystal Structure of Mo2Cl4(NHEt2)4: A Quadruply-Bonded Dimolybdenum Compound with Diethylamine Ligands
F. Albert Cotton; Evgeny V. Dikarev; Santiago Herrero; Inorganic Chemistry 37 (1998) 5862–5868; doi:10.1021/ic980702d

data_4323139
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II). 1. Preparation,
 Characterization, and Crystal Structure of Mo2Cl4(NHEt2)4: A
 Quadruply-Bonded Dimolybdenum Compound with Diethylamine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5862
_journal_page_last               5868
_journal_paper_doi               10.1021/ic980702d
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 [N H2 (C2 H5)2][Mo2 Cl7 (N H (C2 H5)2)2], C7H8
;
_chemical_formula_structural
;
 [NHEt2H][Mo2(\m-Cl)3Cl4(NEt2H)2],C7H8
;
_chemical_formula_sum            'C19 H42 Cl7 Mo2 N3'
_chemical_formula_weight         752.59
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Diethylammonium gauche-tris(\m2-chloro)-tetrachloro-
 -bis(diethylamine)-di-molybdenum(III), toluene solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.68(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.847(5)
_cell_length_b                   10.448(4)
_cell_length_c                   22.091(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      15
_cell_volume                     3174.3(18)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_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      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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5579
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.8264
_exptl_absorpt_correction_type   'empirical, via \y scans'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_obs          0.0289
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+1.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0788
_refine_ls_wR_factor_obs         0.0732
_reflns_number_observed          4650
_reflns_number_total             5579
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980702d_4.cif
_cod_data_source_block           '[NH2Et2][Mo2Cl7(NHEt2)2],C7H8'
_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 1673 2011-04-08 12:14:43Z 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^)+(0.0406P)^2^+1.1279P] 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^)+(0.0406P)^2^+1.1279P] 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        3174(2)
_cod_database_code               4323139