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_4323140
_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]2 [Mo Cl5 (N H (C2 H5)2)]
;
_chemical_formula_structural     '[NH2Et2]2[MoCl5(NHEt2)]'
_chemical_formula_sum            'C12 H35 Cl5 Mo N3'
_chemical_formula_weight         494.62
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(diethylammonium) pentachloro-diethylamine-molybdenum(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                 95.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.710(2)
_cell_length_b                   12.363(2)
_cell_length_c                   30.272(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14.48
_cell_measurement_theta_min      10.92
_cell_volume                     4359.5(14)
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            6212
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.758
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.246
_refine_ls_goodness_of_fit_obs   1.365
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5869
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.245
_refine_ls_restrained_S_obs      1.364
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_obs          0.0600
_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^)+(0.0221P)^2^+33.0239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1486
_refine_ls_wR_factor_obs         0.1374
_reflns_number_observed          4282
_reflns_number_total             5869
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980702d_5.cif
_cod_data_source_block           '[NH2Et2]2[MoCl5(NHEt2)]'
_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^)+(0.0221P)^2^+33.0239P] 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^)+(0.0221P)^2^+33.0239P] 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        4360(1)
_cod_database_code               4323140