#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:51:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332486.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_4332486
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         'C24 H40 Mo2 N12 O'
_chemical_formula_sum            'C24 H40 Mo2 N12 O'
_chemical_formula_weight         704.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 109.097(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.604(2)
_cell_length_b                   24.081(5)
_cell_length_c                   11.473(2)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.4405
_cell_measurement_theta_min      2.272
_cell_volume                     2768.5(9)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ω-scan
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19290
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.8314
_exptl_absorpt_correction_T_min  0.7079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0271
_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)+(0.0275P)²+1.6713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                5252
_reflns_number_total             6322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060449esup1.cif
_cod_data_source_block           1thf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        2768.6(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332486
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-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
Mo1 Mo 0.405692(19) 0.072794(9) 0.303937(19) 0.02276(6) Uani 1 1 d .
Mo2 Mo 0.247105(19) 0.127079(9) 0.203118(18) 0.02199(6) Uani 1 1 d .
N7 N 0.55104(19) 0.13873(9) 0.36036(19) 0.0269(4) Uani 1 1 d .
N10 N 0.3550(2) 0.07840(9) 0.47190(19) 0.0291(5) Uani 1 1 d .
N2 N 0.1033(2) 0.06019(9) 0.1577(2) 0.0292(5) Uani 1 1 d .
N5 N 0.2910(2) 0.11758(9) 0.03346(19) 0.0280(5) Uani 1 1 d .
N11 N 0.1860(2) 0.14137(9) 0.36293(19) 0.0284(5) Uani 1 1 d .
N1 N 0.2807(2) -0.00051(9) 0.2611(2) 0.0309(5) Uani 1 1 d .
N9 N 0.6028(2) 0.22485(9) 0.30169(19) 0.0275(4) Uani 1 1 d .
N8 N 0.3818(2) 0.19820(8) 0.23680(19) 0.0266(4) Uani 1 1 d .
C11 C 0.6966(2) 0.14406(11) 0.4026(2) 0.0299(5) Uani 1 1 d .
H11A H 0.7385 0.1095 0.3887 0.036 Uiso 1 1 calc R
H11B H 0.7309 0.1532 0.4906 0.036 Uiso 1 1 calc R
N4 N 0.4757(2) 0.06268(9) 0.1475(2) 0.0281(5) Uani 1 1 d .
C5 C -0.0427(2) 0.05235(12) 0.1164(2) 0.0321(6) Uani 1 1 d .
H5A H -0.0795 0.0511 0.0262 0.039 Uiso 1 1 calc R
H5B H -0.0861 0.0825 0.1464 0.039 Uiso 1 1 calc R
C19 C 0.0506(3) 0.11866(12) 0.4844(3) 0.0353(6) Uani 1 1 d .
H19A H 0.0076 0.1362 0.5387 0.042 Uiso 1 1 calc R
H19B H 0.0002 0.0854 0.4468 0.042 Uiso 1 1 calc R
N12 N 0.1896(2) 0.10560(10) 0.55019(19) 0.0300(5) Uani 1 1 d .
C8 C 0.4010(2) 0.08918(10) 0.0478(2) 0.0259(5) Uani 1 1 d .
C18 C 0.2494(2) 0.10985(11) 0.4576(2) 0.0269(5) Uani 1 1 d .
C13 C 0.5054(2) 0.18559(10) 0.3024(2) 0.0241(5) Uani 1 1 d .
N6 N 0.4501(2) 0.09113(9) -0.05112(19) 0.0309(5) Uani 1 1 d .
C3 C 0.1550(2) 0.01159(11) 0.2004(2) 0.0280(5) Uani 1 1 d .
C4 C -0.0627(3) -0.00396(12) 0.1734(3) 0.0393(7) Uani 1 1 d .
H4A H -0.0763 0.0012 0.2532 0.047 Uiso 1 1 calc R
H4B H -0.1383 -0.0246 0.1181 0.047 Uiso 1 1 calc R
C7 C 0.5933(3) 0.08095(13) 0.0050(3) 0.0401(7) Uani 1 1 d .
H7A H 0.6432 0.1158 0.0258 0.048 Uiso 1 1 calc R
H7B H 0.6283 0.0591 -0.0497 0.048 Uiso 1 1 calc R
C2 C 0.1314(3) -0.06887(12) 0.2894(3) 0.0390(7) Uani 1 1 d .
H2A H 0.1063 -0.1077 0.2691 0.047 Uiso 1 1 calc R
H2B H 0.1127 -0.0587 0.3648 0.047 Uiso 1 1 calc R
C6 C 0.5994(3) 0.04779(11) 0.1226(2) 0.0322(6) Uani 1 1 d .
H6A H 0.6028 0.0078 0.1084 0.039 Uiso 1 1 calc R
H6B H 0.6781 0.0584 0.1920 0.039 Uiso 1 1 calc R
C16 C 0.3692(3) 0.04517(13) 0.5832(2) 0.0361(6) Uani 1 1 d .
H16A H 0.4421 0.0594 0.6537 0.043 Uiso 1 1 calc R
H16B H 0.3873 0.0062 0.5699 0.043 Uiso 1 1 calc R
C14 C 0.5407(3) 0.25519(12) 0.1863(2) 0.0351(6) Uani 1 1 d .
H14A H 0.5614 0.2380 0.1173 0.042 Uiso 1 1 calc R
H14B H 0.5689 0.2942 0.1936 0.042 Uiso 1 1 calc R
C9 C 0.3922(3) 0.14199(12) -0.1168(3) 0.0368(6) Uani 1 1 d .
H9A H 0.3762 0.1388 -0.2056 0.044 Uiso 1 1 calc R
H9B H 0.4488 0.1744 -0.0844 0.044 Uiso 1 1 calc R
C15 C 0.3908(3) 0.24965(11) 0.1711(2) 0.0316(6) Uani 1 1 d .
H15A H 0.3602 0.2816 0.2076 0.038 Uiso 1 1 calc R
H15B H 0.3368 0.2470 0.0837 0.038 Uiso 1 1 calc R
C10 C 0.2598(3) 0.14481(11) -0.0875(2) 0.0319(6) Uani 1 1 d .
H10A H 0.2322 0.1834 -0.0834 0.038 Uiso 1 1 calc R
H10B H 0.1884 0.1250 -0.1501 0.038 Uiso 1 1 calc R
C1 C 0.2791(3) -0.05831(11) 0.3021(3) 0.0359(6) Uani 1 1 d .
H1A H 0.3368 -0.0628 0.3878 0.043 Uiso 1 1 calc R
H1B H 0.3087 -0.0838 0.2498 0.043 Uiso 1 1 calc R
C12 C 0.7238(3) 0.19180(12) 0.3241(3) 0.0336(6) Uani 1 1 d .
H12A H 0.8037 0.2129 0.3697 0.040 Uiso 1 1 calc R
H12B H 0.7331 0.1780 0.2469 0.040 Uiso 1 1 calc R
N3 N 0.0639(2) -0.03197(10) 0.1876(2) 0.0335(5) Uani 1 1 d .
C17 C 0.2344(3) 0.05116(12) 0.6054(3) 0.0370(6) Uani 1 1 d .
H17A H 0.1721 0.0217 0.5638 0.044 Uiso 1 1 calc R
H17B H 0.2454 0.0508 0.6936 0.044 Uiso 1 1 calc R
C20 C 0.0636(2) 0.15946(12) 0.3858(2) 0.0330(6) Uani 1 1 d .
H20A H -0.0138 0.1570 0.3104 0.040 Uiso 1 1 calc R
H20B H 0.0722 0.1978 0.4163 0.040 Uiso 1 1 calc R
O1 O 0.0612(2) 0.19757(10) 0.0957(2) 0.0532(6) Uani 1 1 d .
C1S C -0.0443(3) 0.18863(14) -0.0166(3) 0.0492(8) Uani 1 1 d .
H1SA H -0.0688 0.1493 -0.0264 0.059 Uiso 1 1 calc R
H1SB H -0.0178 0.2004 -0.0870 0.059 Uiso 1 1 calc R
C4S C 0.0458(3) 0.25320(14) 0.1315(3) 0.0532(8) Uani 1 1 d .
H4SA H 0.0882 0.2793 0.0902 0.064 Uiso 1 1 calc R
H4SB H 0.0867 0.2576 0.2209 0.064 Uiso 1 1 calc R
C2S C -0.1598(3) 0.22331(18) -0.0079(4) 0.0661(11) Uani 1 1 d .
H2SA H -0.2031 0.2428 -0.0857 0.079 Uiso 1 1 calc R
H2SB H -0.2262 0.1999 0.0111 0.079 Uiso 1 1 calc R
C3S C -0.1000(4) 0.26353(18) 0.0937(4) 0.0703(11) Uani 1 1 d .
H3SA H -0.1209 0.3018 0.0646 0.084 Uiso 1 1 calc R
H3SB H -0.1334 0.2571 0.1627 0.084 Uiso 1 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
Mo2 Mo1 N7 94.03(6)
Mo2 Mo1 N1 93.49(6)
N7 Mo1 N1 172.48(8)
Mo2 Mo1 N10 93.59(6)
N7 Mo1 N10 92.76(8)
N1 Mo1 N10 86.62(8)
Mo2 Mo1 N4 92.43(6)
N7 Mo1 N4 85.79(8)
N1 Mo1 N4 94.04(8)
N10 Mo1 N4 173.90(8)
Mo1 Mo2 N5 93.41(6)
Mo1 Mo2 N2 92.45(6)
N5 Mo2 N2 92.68(8)
Mo1 Mo2 N11 92.25(6)
N5 Mo2 N11 174.32(8)
N2 Mo2 N11 86.55(8)
Mo1 Mo2 N8 91.75(5)
N5 Mo2 N8 85.47(8)
N2 Mo2 N8 175.50(8)
N11 Mo2 N8 94.89(8)
Mo1 Mo2 O1 175.66(5)
N5 Mo2 O1 89.74(8)
N2 Mo2 O1 90.37(8)
N11 Mo2 O1 84.63(8)
N8 Mo2 O1 85.53(8)
C13 N7 C11 105.4(2)
C13 N7 Mo1 111.69(16)
C11 N7 Mo1 137.34(17)
C18 N10 C16 105.2(2)
C18 N10 Mo1 111.94(16)
C16 N10 Mo1 138.79(18)
C3 N2 C5 105.7(2)
C3 N2 Mo2 113.41(16)
C5 N2 Mo2 139.13(17)
C8 N5 C10 105.5(2)
C8 N5 Mo2 112.73(16)
C10 N5 Mo2 139.08(17)
C18 N11 C20 105.4(2)
C18 N11 Mo2 113.26(16)
C20 N11 Mo2 136.41(16)
C3 N1 C1 105.2(2)
C3 N1 Mo1 112.18(17)
C1 N1 Mo1 140.29(18)
C13 N9 C12 103.79(19)
C13 N9 C14 103.14(19)
C12 N9 C14 122.7(2)
C13 N8 C15 105.6(2)
C13 N8 Mo2 113.07(16)
C15 N8 Mo2 136.01(16)
N7 C11 C12 104.5(2)
C8 N4 C6 105.6(2)
C8 N4 Mo1 113.04(16)
C6 N4 Mo1 138.97(17)
N2 C5 C4 104.5(2)
N12 C19 C20 101.6(2)
C18 N12 C19 102.85(19)
C18 N12 C17 103.2(2)
C19 N12 C17 123.2(2)
N5 C8 N4 127.9(2)
N5 C8 N6 115.6(2)
N4 C8 N6 116.3(2)
N11 C18 N10 128.2(2)
N11 C18 N12 115.5(2)
N10 C18 N12 116.0(2)
N8 C13 N7 128.2(2)
N8 C13 N9 116.0(2)
N7 C13 N9 115.5(2)
C8 N6 C9 104.0(2)
C8 N6 C7 104.3(2)
C9 N6 C7 124.5(2)
N2 C3 N1 128.2(2)
N2 C3 N3 115.9(2)
N1 C3 N3 115.7(2)
N3 C4 C5 101.7(2)
N6 C7 C6 102.1(2)
N3 C2 C1 101.1(2)
N4 C6 C7 104.9(2)
N10 C16 C17 104.8(2)
N9 C14 C15 101.5(2)
N6 C9 C10 100.5(2)
N8 C15 C14 104.6(2)
N5 C10 C9 104.2(2)
N1 C1 C2 104.1(2)
N9 C12 C11 100.80(19)
C3 N3 C2 103.4(2)
C3 N3 C4 104.0(2)
C2 N3 C4 124.3(2)
N12 C17 C16 101.5(2)
N11 C20 C19 103.8(2)
C1S O1 C4S 105.9(2)
C1S O1 Mo2 125.73(19)
C4S O1 Mo2 128.35(18)
O1 C1S C2S 105.7(3)
O1 C4S C3S 106.3(3)
C3S C2S C1S 105.3(3)
C4S C3S C2S 104.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 Mo2 2.1453(4)
Mo1 N7 2.159(2)
Mo1 N1 2.165(2)
Mo1 N10 2.168(2)
Mo1 N4 2.168(2)
Mo2 N5 2.156(2)
Mo2 N2 2.161(2)
Mo2 N11 2.163(2)
Mo2 N8 2.182(2)
Mo2 O1 2.588(2)
N7 C13 1.319(3)
N7 C11 1.465(3)
N10 C18 1.317(3)
N10 C16 1.473(3)
N2 C3 1.317(3)
N2 C5 1.476(3)
N5 C8 1.315(3)
N5 C10 1.471(3)
N11 C18 1.315(3)
N11 C20 1.472(3)
N1 C3 1.319(3)
N1 C1 1.471(3)
N9 C13 1.402(3)
N9 C12 1.460(3)
N9 C14 1.466(3)
N8 C13 1.316(3)
N8 C15 1.470(3)
C11 C12 1.545(4)
N4 C8 1.323(3)
N4 C6 1.476(3)
C5 C4 1.550(4)
C19 N12 1.454(3)
C19 C20 1.538(4)
N12 C18 1.407(3)
N12 C17 1.465(4)
C8 N6 1.396(3)
N6 C9 1.463(3)
N6 C7 1.464(4)
C3 N3 1.401(3)
C4 N3 1.463(3)
C7 C6 1.552(4)
C2 N3 1.456(3)
C2 C1 1.545(4)
C16 C17 1.539(4)
C14 C15 1.547(4)
C9 C10 1.548(4)
O1 C1S 1.419(4)
O1 C4S 1.426(4)
C1S C2S 1.513(5)
C4S C3S 1.484(5)
C2S C3S 1.488(5)
