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_4322035
_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         'Mo Cl3 (N H2 C3 H7)3, 1/6 O C4 H8'
_chemical_formula_structural     mer-MoCl3(NH2n-Pr)3,1/6THF
_chemical_formula_sum            'C9.67 H28.33 Cl3 Mo N3 O0.17'
_chemical_formula_weight         391.64
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Mer-trichloro-tris(propylamine)-molybdenum(III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.32(1)
_cell_angle_beta                 103.21(2)
_cell_angle_gamma                103.48(1)
_cell_formula_units_Z            12
_cell_length_a                   12.370(2)
_cell_length_b                   17.977(2)
_cell_length_c                   25.498(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      17
_cell_volume                     5303.8(17)
_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
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15512
_diffrn_reflns_theta_max         23.01
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9381
_exptl_absorpt_correction_type   'empirical, via \y-scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.686
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         14699
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_obs          0.0551
_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^)+(0.0741P)^2^+22.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1579
_refine_ls_wR_factor_obs         0.1386
_reflns_number_observed          10628
_reflns_number_total             14699
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981289c_3.cif
_cod_data_source_block           MoCl3(NH2Pr)3,1/6THF
_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^)+(0.0741P)^2^+22.3952P] 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^)+(0.0741P)^2^+22.3952P] 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        5304(2)
_cod_database_code               4322035