Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 3. Preparation, Characterization, and Crystal Structure of Mo2Cl4(NH2R)4 (R = Et, Prn, But, Cy): First Quadruply-Bonded Dimolybdenum Compounds with Primary Amine Ligands
F. Albert Cotton; Evgeny V. Dikarev; Santiago Herrero; Inorganic Chemistry 38 (1999) 2649–2654; doi:10.1021/ic981289c

data_4322034
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 3. Preparation,
 Characterization, and Crystal Structure of Mo2Cl4(NH2R)4 (R = Et, Prn,
 But, Cy): First Quadruply-Bonded Dimolybdenum Compounds with Primary
 Amine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2649
_journal_page_last               2654
_journal_paper_doi               10.1021/ic981289c
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Mo2 Cl4 (N H2 (C3 H7))4'
_chemical_formula_structural     1,3,6,8-Mo2Cl4(NH2n-Pr)4
_chemical_formula_sum            'C12 H36 Cl4 Mo2 N4'
_chemical_formula_weight         570.13
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(propylamine))-di-molybdenum(II)
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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            4
_cell_length_a                   13.328(3)
_cell_length_b                   26.639(5)
_cell_length_c                   6.774(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      15.42
_cell_measurement_theta_min      12.48
_cell_volume                     2405.1(10)
_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      153(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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1670
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_type   'empirical, via \y-scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.177
_refine_ls_hydrogen_treatment    'refined on N(1) atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         840
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.173
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_obs          0.0316
_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^)+(0.0399P)^2^+0.6154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0839
_refine_ls_wR_factor_obs         0.0732
_reflns_number_observed          560
_reflns_number_total             840
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981289c_2.cif
_cod_data_source_block           Mo2Cl4(NH2Pr)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^)+(0.0399P)^2^+0.6154P] 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^)+(0.0399P)^2^+0.6154P] 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        2405(1)
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4322034