#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:51:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332492.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332492
loop_
_publ_author_name
'Cotton, F. Albert'
'Murillo, Carlos A.'
'Wang, Xiaoping'
'Wilkinson, Chad C.'
_publ_section_title
;
 Homologues of the Easily Ionized Compound Mo2(hpp)4Containing Smaller
 Bicyclic Guanidinates
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5493
_journal_page_last               5500
_journal_paper_doi               10.1021/ic060449e
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C27 H43 Cl11 Mo2 N12'
_chemical_formula_sum            'C27 H43 Cl11 Mo2 N12'
_chemical_formula_weight         1117.56
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                102.568(3)
_cell_angle_beta                 97.518(3)
_cell_angle_gamma                116.077(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6019(17)
_cell_length_b                   10.0355(18)
_cell_length_c                   13.051(2)
_cell_measurement_reflns_used    2595
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.6735
_cell_measurement_theta_min      2.440
_cell_volume                     1065.1(3)
_computing_cell_refinement       'Bruker SMART'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       /w-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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6260
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.9371
_exptl_absorpt_correction_T_min  0.7342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1176P)²+2.7186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1937
_reflns_number_gt                3085
_reflns_number_total             3704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060449esup1.cif
_cod_data_source_block           5threeCHCl3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332492
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_assembly
_atom_site_disorder_group
Mo1 Mo 0.57355(7) 0.62215(6) 0.55468(4) 0.0383(2) Uani 1 1 d . . .
Cl1 Cl 0.7573(2) 0.9346(2) 0.68528(16) 0.0570(5) Uani 1 1 d . . .
Cl6 Cl 0.5811(5) 0.2425(4) 0.7321(3) 0.1144(11) Uani 1 1 d D . .
C3 C 0.3693(8) 0.4169(7) 0.6663(5) 0.0405(14) Uani 1 1 d . . .
N1 N 0.3220(7) 0.3094(6) 0.5676(4) 0.0424(12) Uani 1 1 d . . .
N2 N 0.4835(7) 0.5626(6) 0.6867(4) 0.0456(13) Uani 1 1 d . . .
C9 C 0.7454(9) 0.4403(8) 0.5635(6) 0.0469(16) Uani 1 1 d . A .
Cl5 Cl 0.5049(7) 0.0741(5) 0.8837(4) 0.171(2) Uani 1 1 d D . .
N4 N 0.6105(7) 0.3298(6) 0.4886(5) 0.0444(13) Uani 1 1 d . . .
N5 N 0.7650(7) 0.5812(7) 0.6121(5) 0.0494(14) Uani 1 1 d . . .
N3 N 0.2911(9) 0.3629(9) 0.7382(6) 0.0642(18) Uani 1 1 d . . .
N6 N 0.8569(9) 0.3950(9) 0.5819(7) 0.072(2) Uani 1 1 d . . .
Cl4 Cl 0.8105(8) 0.3460(7) 0.9357(4) 0.202(3) Uani 1 1 d D . .
C1 C 0.1874(10) 0.1653(9) 0.5671(6) 0.061(2) Uani 1 1 d D . .
H1A H 0.2036 0.0763 0.5374 0.073 Uiso 1 1 calc R . .
H1B H 0.0874 0.1490 0.5226 0.073 Uiso 1 1 calc R . .
C7 C 0.6298(10) 0.1915(10) 0.4482(8) 0.072(2) Uani 1 1 d D . .
H7A H 0.6332 0.1747 0.3719 0.086 Uiso 1 1 calc R A .
H7B H 0.5402 0.0983 0.4539 0.086 Uiso 1 1 calc R . .
C2 C 0.1802(11) 0.1823(12) 0.6839(8) 0.091(3) Uani 1 1 d D . .
H2A H 0.2227 0.1230 0.7149 0.109 Uiso 1 1 calc R . .
H2B H 0.0704 0.1491 0.6909 0.109 Uiso 1 1 calc R . .
C8 C 0.7864(12) 0.2245(11) 0.5188(8) 0.081(3) Uani 1 1 d D A .
H8A H 0.7682 0.1598 0.5673 0.097 Uiso 1 1 calc R . .
H8B H 0.8558 0.2075 0.4749 0.097 Uiso 1 1 calc R . .
C4 C 0.3180(14) 0.4281(14) 0.8460(8) 0.104(4) Uani 1 1 d D . .
H4A H 0.3248 0.3578 0.8856 0.125 Uiso 1 1 calc R . .
H4B H 0.2299 0.4477 0.8603 0.125 Uiso 1 1 calc R . .
C25 C 0.6570(9) 0.1875(9) 0.8333(6) 0.102(4) Uani 1 1 d D . .
H25A H 0.7021 0.1223 0.7998 0.122 Uiso 1 1 calc R . .
C5 C 0.4771(17) 0.5827(14) 0.8835(9) 0.136(5) Uani 1 1 d DU . .
H5A H 0.4707 0.6551 0.9442 0.163 Uiso 1 1 calc R . .
H5B H 0.5635 0.5625 0.9111 0.163 Uiso 1 1 calc R . .
C10 C 0.9976(14) 0.4749(13) 0.6651(9) 0.095(3) Uani 0.57(3) 1 d PD A 1
H10A H 1.0904 0.5134 0.6345 0.114 Uiso 0.57(3) 1 calc PR A 1
H10B H 1.0059 0.4042 0.7037 0.114 Uiso 0.57(3) 1 calc PR A 1
C11 C 0.998(3) 0.610(2) 0.7431(17) 0.081(6) Uani 0.57(3) 1 d PD A 1
H11E H 1.1087 0.6845 0.7852 0.097 Uiso 0.57(3) 1 calc PR A 1
H11F H 0.9361 0.5714 0.7941 0.097 Uiso 0.57(3) 1 calc PR A 1
C12 C 0.929(5) 0.694(6) 0.689(5) 0.070(8) Uani 0.57(3) 1 d PD A 1
H11A H 1.0018 0.7493 0.6481 0.084 Uiso 0.57(3) 1 calc PR A 1
H11B H 0.9210 0.7713 0.7444 0.084 Uiso 0.57(3) 1 calc PR A 1
C6 C 0.5233(14) 0.6635(10) 0.7962(6) 0.085(3) Uani 1 1 d D . .
H6A H 0.4708 0.7277 0.7945 0.102 Uiso 1 1 calc R . .
H6B H 0.6394 0.7341 0.8189 0.102 Uiso 1 1 calc R . .
C10A C 0.9976(14) 0.4749(13) 0.6651(9) 0.095(3) Uani 0.43(3) 1 d PD A 2
H10C H 1.0860 0.4674 0.6392 0.114 Uiso 0.43(3) 1 calc PR A 2
H10D H 0.9835 0.4324 0.7261 0.114 Uiso 0.43(3) 1 calc PR A 2
C11A C 1.031(4) 0.641(2) 0.699(3) 0.081(6) Uani 0.43(3) 1 d PD A 2
H11G H 1.0793 0.6898 0.6458 0.097 Uiso 0.43(3) 1 calc PR A 2
H11H H 1.1111 0.6961 0.7690 0.097 Uiso 0.43(3) 1 calc PR A 2
C12A C 0.890(6) 0.669(9) 0.709(7) 0.070(8) Uani 0.43(3) 1 d PD A 2
H11C H 0.8513 0.6379 0.7703 0.084 Uiso 0.43(3) 1 calc PR A 2
H11D H 0.9243 0.7800 0.7231 0.084 Uiso 0.43(3) 1 calc PR A 2
Cl3 Cl 1.1519(9) 1.0268(10) 0.9559(5) 0.294(6) Uani 1 1 d D . .
Cl2 Cl 0.9467(13) 0.7880(12) 1.0036(6) 0.164(4) Uani 0.50 1 d PD . .
C26 C 1.0325(18) 0.9867(16) 1.0445(12) 0.142(14) Uani 0.50 1 d PD . .
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
N4 Mo1 N1 93.5(2) 2_666 2_666
N4 Mo1 N2 89.1(2) 2_666 .
N1 Mo1 N2 176.0(2) 2_666 .
N4 Mo1 N5 175.6(2) 2_666 .
N1 Mo1 N5 89.7(2) 2_666 .
N2 Mo1 N5 87.5(2) . .
N4 Mo1 Mo1 90.87(16) 2_666 2_666
N1 Mo1 Mo1 90.75(15) 2_666 2_666
N2 Mo1 Mo1 92.25(15) . 2_666
N5 Mo1 Mo1 92.16(16) . 2_666
N4 Mo1 Cl1 87.80(16) 2_666 .
N1 Mo1 Cl1 87.39(15) 2_666 .
N2 Mo1 Cl1 89.68(15) . .
N5 Mo1 Cl1 89.28(16) . .
Mo1 Mo1 Cl1 177.64(5) 2_666 .
N2 C3 N3 124.3(7) . .
N2 C3 N1 121.3(6) . .
N3 C3 N1 114.4(6) . .
C3 N1 C1 108.6(6) . .
C3 N1 Mo1 118.9(4) . 2_666
C1 N1 Mo1 132.0(5) . 2_666
C3 N2 C6 115.1(6) . .
C3 N2 Mo1 116.5(4) . .
C6 N2 Mo1 128.3(5) . .
N5 C9 N4 122.0(6) . .
N5 C9 N6 124.7(7) . .
N4 C9 N6 113.3(7) . .
C9 N4 C7 108.5(6) . .
C9 N4 Mo1 119.5(5) . 2_666
C7 N4 Mo1 132.0(5) . 2_666
C9 N5 C12A 115(2) . .
C9 N5 C12 114.4(17) . .
C9 N5 Mo1 115.3(4) . .
C12A N5 Mo1 128(2) . .
C12 N5 Mo1 129.8(15) . .
C3 N3 C4 131.1(8) . .
C3 N3 C2 106.9(7) . .
C4 N3 C2 120.3(8) . .
C9 N6 C10 126.1(8) . .
C9 N6 C8 109.2(7) . .
C10 N6 C8 122.7(7) . .
N1 C1 C2 106.5(6) . .
N4 C7 C8 106.2(7) . .
C1 C2 N3 101.1(6) . .
N6 C8 C7 101.8(6) . .
N3 C4 C5 107.9(10) . .
Cl5 C25 Cl4 111.5(5) . .
Cl5 C25 Cl6 110.3(5) . .
Cl4 C25 Cl6 112.2(5) . .
C6 C5 C4 115.7(10) . .
N6 C10 C11 109.9(12) . .
C10 C11 C12 114(3) . .
C11 C12 N5 111(3) . .
N2 C6 C5 116.6(8) . .
N5 C12A C11A 110(5) . .
C26 Cl3 C26 47.4(11) 2_777 .
C26 Cl3 Cl2 68.6(8) . 2_777
C26 Cl2 Cl3 45.0(6) . 2_777
C26 C26 Cl2 102.0(16) 2_777 .
C26 C26 Cl3 66.5(12) 2_777 2_777
Cl2 C26 Cl3 90.2(8) . 2_777
C26 C26 Cl3 66.1(10) 2_777 .
Cl2 C26 Cl3 99.3(9) . .
Cl3 C26 Cl3 132.6(11) 2_777 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 N4 2.069(6) 2_666
Mo1 N1 2.077(6) 2_666
Mo1 N2 2.111(6) .
Mo1 N5 2.132(6) .
Mo1 Mo1 2.2243(10) 2_666
Mo1 Cl1 2.8059(19) .
Cl6 C25 1.731(7) .
C3 N2 1.325(9) .
C3 N3 1.337(9) .
C3 N1 1.356(9) .
N1 C1 1.453(9) .
N2 C6 1.450(9) .
C9 N5 1.334(9) .
C9 N4 1.341(9) .
C9 N6 1.349(10) .
Cl5 C25 1.726(7) .
N4 C7 1.473(9) .
N5 C12A 1.42(8) .
N5 C12 1.52(6) .
N3 C4 1.353(12) .
N3 C2 1.571(13) .
N6 C10 1.390(12) .
N6 C8 1.511(12) .
Cl4 C25 1.728(7) .
C1 C2 1.510(9) .
C7 C8 1.512(9) .
C4 C5 1.5395(11) .
C5 C6 1.5391(11) .
C10 C11 1.505(10) .
C11 C12 1.508(11) .
C11A C12A 1.509(11) .
Cl3 C26 1.720(9) .
Cl2 C26 1.708(9) .
