#------------------------------------------------------------------------------
#$Date: 2016-03-22 22:57:19 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179040 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/02/4300246.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4300246
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Santiago Herrero'
_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/[σ²(Fo²)+(0.0222P)²+18.2291P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0199(3) 0.0197(3) 0.0169(3) 0.000 0.000 -0.0018(2)
Mo2 0.0158(3) 0.0209(3) 0.0159(3) 0.000 0.000 0.0010(2)
P1 0.0218(5) 0.0314(6) 0.0262(6) 0.0020(4) -0.0004(4) 0.0063(4)
Cl1 0.0302(5) 0.0329(5) 0.0267(5) -0.0055(4) 0.0051(4) 0.0036(4)
Cl2 0.0310(5) 0.0334(6) 0.0329(6) 0.0109(4) 0.0022(4) -0.0060(4)
N1 0.024(2) 0.023(2) 0.025(2) 0.0009(15) -0.0048(15) -0.0008(14)
C1 0.026(2) 0.047(3) 0.042(3) -0.001(2) -0.001(2) 0.005(2)
C2 0.048(3) 0.033(3) 0.061(3) 0.005(2) 0.000(2) 0.010(2)
C3 0.045(3) 0.074(3) 0.030(3) 0.012(2) -0.001(2) 0.015(2)
C4 0.029(2) 0.032(2) 0.040(2) 0.001(2) 0.009(2) -0.001(2)
C5 0.035(3) 0.039(3) 0.056(3) 0.011(2) 0.003(2) -0.014(2)
C6 0.047(3) 0.024(2) 0.073(4) 0.007(2) -0.016(2) -0.011(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.5000 0.7500 0.77275(3) 0.0188(2) Uani 1 d S .
Mo2 Mo 0.5000 0.7500 0.90818(3) 0.0175(2) Uani 1 d S .
P1 P 0.62008(5) 0.67840(6) 0.94278(6) 0.0265(3) Uani 1 d . .
Cl1 Cl 0.60646(5) 0.67891(5) 0.71773(6) 0.0299(2) Uani 1 d . .
Cl2 Cl 0.43718(5) 0.63668(5) 0.95517(6) 0.0324(3) Uani 1 d . .
N1 N 0.5619(2) 0.8581(2) 0.7492(2) 0.0240(7) Uani 1 d . .
H1A H 0.5422(23) 0.8707(23) 0.7073(27) 0.029 Uiso 1 d . .
H1B H 0.5467(23) 0.8850(23) 0.7868(27) 0.029 Uiso 1 d . .
C1 C 0.7111(2) 0.7160(3) 0.9098(3) 0.0381(10) Uani 1 d . .
H1C H 0.7161(7) 0.7675(6) 0.9297(15) 0.057 Uiso 1 calc R .
H1D H 0.7146(7) 0.7150(15) 0.8481(3) 0.057 Uiso 1 calc R .
H1E H 0.7511(2) 0.6854(10) 0.9339(15) 0.057 Uiso 1 calc R .
C2 C 0.6258(3) 0.5791(2) 0.9143(3) 0.0471(12) Uani 1 d . .
H2A H 0.6243(18) 0.5740(3) 0.8528(3) 0.071 Uiso 1 calc R .
H2B H 0.5836(10) 0.5523(4) 0.9393(17) 0.071 Uiso 1 calc R .
H2C H 0.6727(8) 0.5582(5) 0.9357(18) 0.071 Uiso 1 calc R .
C3 C 0.6282(3) 0.6772(3) 1.0587(3) 0.0496(12) Uani 1 d . .
H3A H 0.5838(9) 0.6537(17) 1.0830(3) 0.074 Uiso 1 calc R .
H3B H 0.6325(19) 0.7285(3) 1.0797(3) 0.074 Uiso 1 calc R .
H3C H 0.6727(11) 0.6488(16) 1.0750(3) 0.074 Uiso 1 calc R .
C4 C 0.6448(2) 0.8633(2) 0.7496(3) 0.0340(10) Uani 1 d . .
H4A H 0.6651(2) 0.8292(2) 0.7062(3) 0.041 Uiso 1 calc R .
H4B H 0.6636(2) 0.8465(2) 0.8052(3) 0.041 Uiso 1 calc R .
C5 C 0.6736(2) 0.9422(2) 0.7326(3) 0.0434(11) Uani 1 d . .
H5A H 0.6520(2) 0.9602(2) 0.6788(3) 0.052 Uiso 1 calc R .
H5B H 0.7284(2) 0.9403(2) 0.7257(3) 0.052 Uiso 1 calc R .
C6 C 0.6549(3) 0.9984(2) 0.8021(3) 0.0481(12) Uani 1 d . .
H6A H 0.6722(16) 1.0481(4) 0.7854(9) 0.072 Uiso 1 calc R .
H6B H 0.6797(14) 0.9836(10) 0.8546(6) 0.072 Uiso 1 calc R .
H6C H 0.6008(3) 0.9996(13) 0.8109(14) 0.072 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo2 Mo1 N1 99.51(9) . 6_564 n
Mo2 Mo1 N1 99.51(9) . . y
N1 Mo1 N1 161.0(2) 6_564 . y
Mo2 Mo1 Cl1 110.82(2) . 6_564 n
N1 Mo1 Cl1 90.25(9) 6_564 6_564 n
N1 Mo1 Cl1 83.01(9) . 6_564 y
Mo2 Mo1 Cl1 110.82(2) . . y
N1 Mo1 Cl1 83.01(9) 6_564 . n
N1 Mo1 Cl1 90.25(9) . . y
Cl1 Mo1 Cl1 138.36(5) 6_564 . y
Mo1 Mo2 Cl2 107.79(3) . 6_564 n
Mo1 Mo2 Cl2 107.79(3) . . y
Cl2 Mo2 Cl2 144.42(5) 6_564 . y
Mo1 Mo2 P1 102.35(2) . . y
Cl2 Mo2 P1 87.93(3) 6_564 . y
Cl2 Mo2 P1 84.57(3) . . y
Mo1 Mo2 P1 102.35(2) . 6_564 n
Cl2 Mo2 P1 84.57(3) 6_564 6_564 n
Cl2 Mo2 P1 87.93(3) . 6_564 n
P1 Mo2 P1 155.30(5) . 6_564 y
C2 P1 C1 103.6(2) . . n
C2 P1 C3 103.2(2) . . n
C1 P1 C3 102.6(2) . . n
C2 P1 Mo2 118.6(2) . . n
C1 P1 Mo2 119.99(15) . . n
C3 P1 Mo2 106.6(2) . . n
C4 N1 Mo1 122.9(2) . . n
N1 C4 C5 113.2(3) . . n
C4 C5 C6 114.0(4) . . n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo2 2.1250(6) . y
Mo1 N1 2.240(3) 6_564 n
Mo1 N1 2.240(3) . y
Mo1 Cl1 2.4292(9) 6_564 n
Mo1 Cl1 2.4292(9) . y
Mo2 Cl2 2.4135(10) 6_564 n
Mo2 Cl2 2.4135(9) . y
Mo2 P1 2.5385(10) . y
Mo2 P1 2.5385(10) 6_564 n
P1 C2 1.819(4) . n
P1 C1 1.822(4) . n
P1 C3 1.825(4) . n
N1 C4 1.473(5) . n
C4 C5 1.514(6) . n
C5 C6 1.514(6) . n
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 Mo2 Mo1 Cl1 2.93(3) . . . . y
Cl2 Mo2 Mo1 N1 0.81(9) . . . 6_564 y
P1 Mo2 Mo1 Cl1 2.93(3) 6_564 . . 6_564 n
Cl2 Mo2 Mo1 N1 0.81(9) 6_564 . . . n
Mo1 Mo2 N1 H1A 44.7(40) . . . . n
Mo1 Mo2 N1 H1B 141.9(31) . . . . n
Mo1 Mo2 N1 C4 -116.5(3) . . . . n
