Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 6. Stepwise Substitution of Amines by Tertiary Phosphines and Vice Versa: Stereochemical Hysteresis
F. Albert Cotton; Evgeny V. Dikarev; Santiago Herrero; Inorganic Chemistry 39 (2000) 609–616; doi:10.1021/ic9913684

data_4300246
_publ_section_title
;
Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 6. Stepwise
Substitution of Amines by Tertiary Phosphines and Vice Versa:
Stereochemical Hysteresis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              609
_journal_page_last               616
_journal_paper_doi               10.1021/ic9913684
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Mo2 Cl4 (N H2 C3 H7)2 (P (C H3)3)2'
_chemical_formula_structural     alpha-Mo2Cl4(NH2n-Pr)2(PMe3)2
_chemical_formula_sum            'C12 H36 Cl4 Mo2 N2 P2'
_chemical_formula_weight         604.05
_chemical_melting_point          ?
_chemical_name_systematic
; 
 1,1,2,2-bis(n-propylamine)-bis(trimethylphosphine)-tetrachloro-
 -di-molybdenum (II, II)
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/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            8
_cell_length_a                   17.737(2)
_cell_length_b                   17.737(2)
_cell_length_c                   15.6915(6)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     4936.6(8)
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11155
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.88
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.175
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_hydrogen_treatment    'refined on N atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_obs          0.0276
_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^)+(0.0222P)^2^+18.2291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0670
_refine_ls_wR_factor_obs         0.0625
_reflns_number_observed          1472
_reflns_number_total             1653
_reflns_observed_criterion       >2sigma(I)
_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.

'_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^)+(0.0222P)^2^+18.2291P] 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^)+(0.0222P)^2^+18.2291P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4300246