#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:52:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178921 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/50/4115010.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_4115010
loop_
_publ_author_name
'F. Albert Cotton'
'Lee M. Daniels'
'Carlos A. Murillo'
'Daren J. Timmons'
'Chad C. Wilkinson'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, P.O. Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 The Extraordinary Ability of Guanidinate Derivatives to Stabilize Higher
 Oxidation Numbers in Dimetal Units by Modification of Redox Potentials:
 Structures of Mo25+ and Mo26+ Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9249
_journal_page_last               9256
_journal_paper_doi               10.1021/ja0266464
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         Mo2(hpp)4Cl.2CH2Cl2
_chemical_formula_sum            'C30 H52 Cl5 Mo2 N12'
_chemical_formula_weight         949.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6912(8)
_cell_length_b                   13.6912(8)
_cell_length_c                   20.4755(12)
_cell_measurement_reflns_used    6054
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.895
_cell_volume                     3838.1(4)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ω-scans
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0080
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21709
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.578664
_exptl_absorpt_correction_T_min  0.502988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00136(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0260P)²+2.7795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                1936
_reflns_number_total             2223
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0266464_s2_3.cif
_cod_data_source_block           compound22CH2CL2
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               4115010
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.2500 0.2500 0.409065(12) 0.02460(9) Uani 1 4 d SD .
Mo2 Mo 0.2500 0.2500 0.512997(12) 0.02218(9) Uani 1 4 d SD .
Cl1 Cl 0.2500 0.2500 0.65161(4) 0.0307(2) Uani 0.9731(19) 4 d SPD .
Cl1A Cl 0.2500 0.2500 0.27036(16) 0.0307(2) Uani 0.0269(19) 4 d SPD 1
N1 N 0.19608(11) 0.10657(11) 0.40220(6) 0.0295(3) Uani 1 1 d . .
N2 N 0.19485(10) 0.10226(10) 0.51416(6) 0.0255(3) Uani 1 1 d . .
N3 N 0.15409(12) -0.04085(11) 0.45470(7) 0.0336(3) Uani 1 1 d . .
C1 C 0.17177(15) 0.06051(14) 0.34017(8) 0.0375(4) Uani 1 1 d . .
H1A H 0.2029 0.0965 0.3044 0.045 Uiso 1 1 calc R .
H1B H 0.1009 0.0627 0.3335 0.045 Uiso 1 1 calc R .
C2 C 0.20590(16) -0.04418(15) 0.33939(10) 0.0438(5) Uani 1 1 d . .
H2A H 0.2768 -0.0470 0.3455 0.053 Uiso 1 1 calc R .
H2B H 0.1899 -0.0746 0.2974 0.053 Uiso 1 1 calc R .
C3 C 0.15502(17) -0.09748(14) 0.39424(9) 0.0431(5) Uani 1 1 d . .
H3A H 0.0876 -0.1118 0.3812 0.052 Uiso 1 1 calc R .
H3B H 0.1882 -0.1598 0.4020 0.052 Uiso 1 1 calc R .
C4 C 0.18125(12) 0.05551(12) 0.45735(7) 0.0256(3) Uani 1 1 d . .
C5 C 0.12139(17) -0.09568(14) 0.51142(9) 0.0414(5) Uani 1 1 d . .
H5A H 0.1717 -0.1430 0.5239 0.050 Uiso 1 1 calc R .
H5B H 0.0619 -0.1319 0.5004 0.050 Uiso 1 1 calc R .
C6 C 0.10111(15) -0.02817(14) 0.56819(9) 0.0396(4) Uani 1 1 d . .
H6A H 0.0958 -0.0661 0.6086 0.048 Uiso 1 1 calc R .
H6B H 0.0392 0.0061 0.5612 0.048 Uiso 1 1 calc R .
C7 C 0.18343(13) 0.04500(13) 0.57405(8) 0.0307(4) Uani 1 1 d . .
H7A H 0.1701 0.0891 0.6107 0.037 Uiso 1 1 calc R .
H7B H 0.2445 0.0104 0.5833 0.037 Uiso 1 1 calc R .
Cl4 Cl -0.04069(9) -0.42598(8) 0.25138(12) 0.0581(4) Uani 0.50 1 d P .
C8 C -0.0383(3) -0.2978(3) 0.2476(2) 0.0431(9) Uani 0.50 1 d P .
Cl2 Cl 0.08219(7) -0.2500 0.2500 0.0775(3) Uani 1 2 d S .
H8 H -0.069(2) -0.257(2) 0.2080(14) 0.090(10) Uiso 1 1 d . .
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'
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
N1 Mo1 N1 89.745(5) 2 3 ?
N1 Mo1 N1 89.744(5) 2 4 ?
N1 Mo1 N1 172.33(7) 3 4 ?
N1 Mo1 N1 172.33(7) 2 . y
N1 Mo1 N1 89.742(5) 3 . y
N1 Mo1 N1 89.744(5) 4 . ?
N1 Mo1 Mo2 93.83(4) 2 . ?
N1 Mo1 Mo2 93.83(4) 3 . ?
N1 Mo1 Mo2 93.83(4) 4 . ?
N1 Mo1 Mo2 93.83(4) . . y
N1 Mo1 Cl1A 86.17(4) 2 . ?
N1 Mo1 Cl1A 86.17(4) 3 . ?
N1 Mo1 Cl1A 86.17(4) 4 . ?
N1 Mo1 Cl1A 86.17(4) . . y
Mo2 Mo1 Cl1A 180.0 . . y
Mo1 Mo2 N2 90.63(3) . 2 ?
Mo1 Mo2 N2 90.63(3) . 3 ?
N2 Mo2 N2 89.995(1) 2 3 ?
Mo1 Mo2 N2 90.63(3) . . y
N2 Mo2 N2 178.73(7) 2 . y
N2 Mo2 N2 89.992(1) 3 . y
Mo1 Mo2 N2 90.63(3) . 4 ?
N2 Mo2 N2 89.993(1) 2 4 ?
N2 Mo2 N2 178.74(7) 3 4 ?
N2 Mo2 N2 89.992(1) . 4 ?
Mo1 Mo2 Cl1 180.0 . . y
N2 Mo2 Cl1 89.37(3) 2 . ?
N2 Mo2 Cl1 89.37(3) 3 . ?
N2 Mo2 Cl1 89.37(3) . . y
N2 Mo2 Cl1 89.37(3) 4 . ?
Cl1A Cl1A Mo1 180.0 5 . ?
C4 N1 C1 118.23(15) . . ?
C4 N1 Mo1 118.87(11) . . ?
C1 N1 Mo1 122.88(11) . . ?
C4 N2 C7 117.15(14) . . ?
C4 N2 Mo2 119.09(11) . . ?
C7 N2 Mo2 123.25(10) . . ?
C4 N3 C5 123.28(14) . . ?
C4 N3 C3 122.79(15) . . ?
C5 N3 C3 113.93(15) . . ?
N1 C1 C2 110.48(16) . . ?
C1 C2 C3 107.98(16) . . ?
N3 C3 C2 112.20(15) . . ?
N2 C4 N1 117.38(15) . . ?
N2 C4 N3 122.07(15) . . ?
N1 C4 N3 120.54(14) . . ?
N3 C5 C6 110.82(15) . . ?
C5 C6 C7 109.22(16) . . ?
N2 C7 C6 111.58(14) . . ?
Cl4 Cl4 C8 135.46(17) 8_445 . ?
C8 C8 Cl4 173.2(5) 6_545 . ?
C8 C8 Cl2 68.32(14) 6_545 . ?
Cl4 C8 Cl2 112.6(2) . . ?
C8 Cl2 C8 43.4(3) . 6_545 ?
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 N1 2.1026(15) 2 ?
Mo1 N1 2.1026(15) 3 ?
Mo1 N1 2.1026(15) 4 ?
Mo1 N1 2.1026(15) . y
Mo1 Mo2 2.1281(4) . y
Mo1 Cl1A 2.840(3) . y
Mo2 N2 2.1592(14) 2 ?
Mo2 N2 2.1592(14) 3 ?
Mo2 N2 2.1592(14) . y
Mo2 N2 2.1593(14) 4 ?
Mo2 Cl1 2.8381(9) . y
Cl1A Cl1A 0.834(6) 5 ?
N1 C4 1.343(2) . y
N1 C1 1.457(2) . y
N2 C4 1.341(2) . y
N2 C7 1.464(2) . y
N3 C4 1.372(2) . y
N3 C5 1.453(2) . y
N3 C3 1.461(2) . y
C1 C2 1.508(3) . ?
C2 C3 1.510(3) . ?
C5 C6 1.511(3) . ?
C6 C7 1.513(3) . ?
Cl4 Cl4 0.648(2) 8_445 ?
Cl4 C8 1.757(5) . ?
C8 C8 1.312(9) 6_545 ?
C8 Cl2 1.776(4) . ?
Cl2 C8 1.776(4) 6_545 ?
