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_4323137
_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         'Mo2 Cl4 (N H (C2 H5)2 )4'
_chemical_formula_structural     1,3,6,8-Mo2Cl4(NHEt2)4
_chemical_formula_sum            'C16 H44 Cl4 Mo2 N4'
_chemical_formula_weight         626.23
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(diethylamine))-di-molybdenum(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.72(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.846(1)
_cell_length_b                   7.044(1)
_cell_length_c                   19.868(3)
_cell_measurement_reflns_used    243
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     2558.5(7)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_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      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4794
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         3.10
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_obs          0.0298
_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^)+(0.0311P)^2^+7.1527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0706
_refine_ls_wR_factor_obs         0.0676
_reflns_number_observed          1568
_reflns_number_total             1671
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980702d_2.cif
_cod_data_source_block           Mo2Cl4(NHEt2)4
_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^)+(0.0311P)^2^+7.1527P] 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^)+(0.0311P)^2^+7.1527P] 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        2558.5(5)
_cod_database_code               4323137