#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:45:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179763 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/59/7005965.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_7005965
loop_
_publ_author_name
'Cotton, F. Albert'
'Murillo, Carlos A.'
'Wang, Xiaoping'
'Wilkinson, Chad C.'
_publ_section_title
;
 Increasing the solubility of strong reducing agents containing
 Mo(2)(4+) units and alkyl-substituted guanidinate ligands.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3943
_journal_page_last               3951
_journal_paper_doi               10.1039/b707201e
_journal_year                    2007
_chemical_formula_moiety         'C11 H22 N3, H1 C1 O3'
_chemical_formula_sum            'C12 H23 N3 O3'
_chemical_formula_weight         257.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.038(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.853(3)
_cell_length_b                   15.973(4)
_cell_length_c                   13.067(3)
_cell_measurement_reflns_used    3571
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.048
_cell_measurement_theta_min      2.36
_cell_volume                     2855.5(12)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12778
_diffrn_reflns_theta_full        27.79
_diffrn_reflns_theta_max         27.79
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.9657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         12845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0604
_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)+(0.0581P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                5634
_reflns_number_total             12845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b707201e.txt
_cod_data_source_block           H2TMhppHCO3
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2855.6(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005965
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.66377(9) 0.07410(7) 0.45921(9) 0.0390(3) Uani 1 1 d . . .
H3A H 0.7217 0.0847 0.4825 0.059 Uiso 1 1 calc R . .
O1A O 0.97655(10) 0.16481(8) 0.60413(11) 0.0494(4) Uani 1 1 d . . .
O3A O 0.84129(10) 0.23171(7) 0.53986(10) 0.0471(4) Uani 1 1 d . . .
H3AC H 0.7862 0.2211 0.5075 0.071 Uiso 1 1 calc R . .
O2A O 0.84552(10) 0.09185(8) 0.53575(10) 0.0436(4) Uani 1 1 d . . .
O2 O 0.66482(10) 0.21319(8) 0.43768(10) 0.0439(4) Uani 1 1 d . . .
O1 O 0.53266(10) 0.13779(8) 0.37706(11) 0.0485(4) Uani 1 1 d . . .
N3 N 0.43148(11) 0.84367(9) 0.33199(12) 0.0353(4) Uani 1 1 d . . .
N3A N 1.08461(11) 0.88051(9) 0.69911(12) 0.0364(4) Uani 1 1 d . . .
N2 N 0.56896(12) 0.91464(10) 0.41142(12) 0.0415(4) Uani 1 1 d . . .
H2A H 0.5999 0.9621 0.4213 0.050 Uiso 1 1 calc R . .
C4 C 0.47711(15) 0.91514(12) 0.36168(14) 0.0334(5) Uani 1 1 d . . .
N1 N 0.43418(12) 0.98890(9) 0.33815(12) 0.0389(4) Uani 1 1 d . . .
H1A H 0.4679 1.0345 0.3526 0.047 Uiso 1 1 calc R . .
C4A C 1.04111(15) 0.94991(12) 0.65731(14) 0.0349(5) Uani 1 1 d . . .
C5A C 1.18676(14) 0.88068(12) 0.74763(15) 0.0399(5) Uani 1 1 d . . .
H5AA H 1.2278 0.8655 0.6959 0.048 Uiso 1 1 calc R . .
H5AB H 1.1964 0.8384 0.8026 0.048 Uiso 1 1 calc R . .
N2A N 1.08770(11) 1.02326(9) 0.66571(12) 0.0378(4) Uani 1 1 d . . .
H2AA H 1.0554 1.0684 0.6449 0.045 Uiso 1 1 calc R . .
C12 C 0.61750(15) 0.14545(12) 0.42261(14) 0.0335(5) Uani 1 1 d . . .
N1A N 0.94891(12) 0.94838(9) 0.61045(12) 0.0421(4) Uani 1 1 d . . .
H1AA H 0.9214 0.9957 0.5898 0.051 Uiso 1 1 calc R . .
C12A C 0.89055(16) 0.16062(12) 0.56137(14) 0.0344(5) Uani 1 1 d . . .
C3 C 0.33087(14) 0.84278(11) 0.27799(14) 0.0389(5) Uani 1 1 d . . .
H3B H 0.2863 0.8363 0.3288 0.047 Uiso 1 1 calc R . .
H3C H 0.3218 0.7945 0.2312 0.047 Uiso 1 1 calc R . .
C2 C 0.30501(14) 0.92258(12) 0.21579(14) 0.0382(5) Uani 1 1 d . . .
C5 C 0.47547(14) 0.76264(11) 0.36407(15) 0.0420(5) Uani 1 1 d . . .
H5A H 0.4516 0.7205 0.3117 0.050 Uiso 1 1 calc R . .
H5B H 0.4548 0.7457 0.4294 0.050 Uiso 1 1 calc R . .
C3A C 1.03543(14) 0.79940(11) 0.68287(16) 0.0431(5) Uani 1 1 d . . .
H3AA H 1.0600 0.7622 0.7407 0.052 Uiso 1 1 calc R . .
H3AB H 1.0512 0.7740 0.6192 0.052 Uiso 1 1 calc R . .
C7A C 1.19055(14) 1.03004(11) 0.70849(15) 0.0402(5) Uani 1 1 d . . .
H7AA H 1.2042 1.0864 0.7367 0.048 Uiso 1 1 calc R . .
H7AB H 1.2300 1.0213 0.6534 0.048 Uiso 1 1 calc R . .
C6A C 1.21873(14) 0.96579(12) 0.79359(14) 0.0391(5) Uani 1 1 d . . .
C1 C 0.33311(15) 0.99549(12) 0.28931(15) 0.0412(5) Uani 1 1 d . . .
H1B H 0.3235 1.0482 0.2508 0.049 Uiso 1 1 calc R . .
H1C H 0.2907 0.9960 0.3427 0.049 Uiso 1 1 calc R . .
C7 C 0.61985(15) 0.83861(12) 0.44990(16) 0.0472(5) Uani 1 1 d . . .
H7A H 0.6065 0.8265 0.5199 0.057 Uiso 1 1 calc R . .
H7B H 0.6905 0.8466 0.4537 0.057 Uiso 1 1 calc R . .
C8 C 0.36170(16) 0.92671(12) 0.12395(15) 0.0491(6) Uani 1 1 d . . .
H8A H 0.4313 0.9260 0.1495 0.074 Uiso 1 1 calc R . .
H8B H 0.3449 0.9779 0.0853 0.074 Uiso 1 1 calc R . .
H8C H 0.3446 0.8789 0.0790 0.074 Uiso 1 1 calc R . .
C2A C 0.92532(15) 0.80707(12) 0.67452(16) 0.0432(5) Uani 1 1 d . . .
C6 C 0.58646(15) 0.76505(12) 0.37850(16) 0.0432(5) Uani 1 1 d . . .
C9 C 0.19464(15) 0.92360(13) 0.17760(16) 0.0524(6) Uani 1 1 d . . .
H9A H 0.1600 0.9209 0.2365 0.079 Uiso 1 1 calc R . .
H9B H 0.1769 0.8757 0.1329 0.079 Uiso 1 1 calc R . .
H9C H 0.1771 0.9748 0.1392 0.079 Uiso 1 1 calc R . .
C9A C 0.89837(16) 0.83404(13) 0.77909(17) 0.0559(6) Uani 1 1 d . . .
H9AA H 0.9203 0.7918 0.8309 0.084 Uiso 1 1 calc R . .
H9AB H 0.8280 0.8404 0.7726 0.084 Uiso 1 1 calc R . .
H9AC H 0.9297 0.8870 0.7999 0.084 Uiso 1 1 calc R . .
C11A C 1.16737(16) 0.98474(14) 0.88702(15) 0.0550(6) Uani 1 1 d . . .
H11A H 1.0971 0.9847 0.8651 0.082 Uiso 1 1 calc R . .
H11B H 1.1879 1.0392 0.9152 0.082 Uiso 1 1 calc R . .
H11C H 1.1846 0.9422 0.9397 0.082 Uiso 1 1 calc R . .
C10A C 1.32985(15) 0.96563(14) 0.82732(16) 0.0543(6) Uani 1 1 d . . .
H10A H 1.3617 0.9536 0.7680 0.081 Uiso 1 1 calc R . .
H10B H 1.3474 0.9231 0.8799 0.081 Uiso 1 1 calc R . .
H10C H 1.3507 1.0201 0.8554 0.081 Uiso 1 1 calc R . .
C1A C 0.89153(15) 0.87273(12) 0.59177(16) 0.0462(5) Uani 1 1 d . . .
H1AB H 0.8979 0.8503 0.5234 0.055 Uiso 1 1 calc R . .
H1AC H 0.8224 0.8857 0.5921 0.055 Uiso 1 1 calc R . .
C8A C 0.87990(17) 0.72267(13) 0.64098(19) 0.0646(7) Uani 1 1 d . . .
H8AA H 0.8980 0.7069 0.5749 0.097 Uiso 1 1 calc R . .
H8AB H 0.8093 0.7267 0.6342 0.097 Uiso 1 1 calc R . .
H8AC H 0.9034 0.6807 0.6925 0.097 Uiso 1 1 calc R . .
C10 C 0.62118(16) 0.77620(13) 0.27352(17) 0.0581(7) Uani 1 1 d . . .
H10D H 0.5953 0.8282 0.2419 0.087 Uiso 1 1 calc R . .
H10E H 0.5981 0.7297 0.2285 0.087 Uiso 1 1 calc R . .
H10F H 0.6920 0.7778 0.2837 0.087 Uiso 1 1 calc R . .
C11 C 0.62627(18) 0.68343(13) 0.4298(2) 0.0700(7) Uani 1 1 d . . .
H11D H 0.6037 0.6772 0.4960 0.105 Uiso 1 1 calc R . .
H11E H 0.6971 0.6847 0.4405 0.105 Uiso 1 1 calc R . .
H11F H 0.6032 0.6366 0.3853 0.105 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 N3 C3 121.48(17) . . ?
C4 N3 C5 121.13(17) . . ?
C3 N3 C5 116.92(15) . . ?
C4A N3A C5A 121.40(17) . . ?
C4A N3A C3A 120.34(18) . . ?
C5A N3A C3A 117.58(15) . . ?
C4 N2 C7 123.15(17) . . ?
N3 C4 N1 121.04(19) . . ?
N3 C4 N2 120.58(18) . . ?
N1 C4 N2 118.30(18) . . ?
C4 N1 C1 122.07(16) . . ?
N1A C4A N2A 118.19(17) . . ?
N1A C4A N3A 120.84(18) . . ?
N2A C4A N3A 120.90(19) . . ?
N3A C5A C6A 112.06(15) . . ?
C4A N2A C7A 122.05(16) . . ?
O1 C12 O2 126.14(18) . . ?
O1 C12 O3 116.53(17) . . ?
O2 C12 O3 117.33(19) . . ?
C4A N1A C1A 123.85(17) . . ?
O1A C12A O2A 124.05(18) . . ?
O1A C12A O3A 118.35(18) . . ?
O2A C12A O3A 117.60(19) . . ?
N3 C3 C2 112.10(15) . . ?
C1 C2 C3 106.74(16) . . ?
C1 C2 C9 109.93(16) . . ?
C3 C2 C9 108.75(16) . . ?
C1 C2 C8 110.45(15) . . ?
C3 C2 C8 110.28(15) . . ?
C9 C2 C8 110.60(17) . . ?
N3 C5 C6 112.38(15) . . ?
N3A C3A C2A 112.27(15) . . ?
N2A C7A C6A 110.83(15) . . ?
C7A C6A C5A 106.80(16) . . ?
C7A C6A C10A 110.04(16) . . ?
C5A C6A C10A 109.17(16) . . ?
C7A C6A C11A 110.54(16) . . ?
C5A C6A C11A 110.29(16) . . ?
C10A C6A C11A 109.95(17) . . ?
N1 C1 C2 110.88(15) . . ?
N2 C7 C6 110.35(17) . . ?
C3A C2A C8A 108.34(16) . . ?
C3A C2A C1A 107.42(15) . . ?
C8A C2A C1A 109.73(18) . . ?
C3A C2A C9A 109.96(18) . . ?
C8A C2A C9A 110.96(16) . . ?
C1A C2A C9A 110.34(16) . . ?
C5 C6 C7 107.38(16) . . ?
C5 C6 C11 108.73(17) . . ?
C7 C6 C11 109.57(18) . . ?
C5 C6 C10 110.20(18) . . ?
C7 C6 C10 110.48(16) . . ?
C11 C6 C10 110.41(17) . . ?
N1A C1A C2A 110.82(17) . . ?
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
O3 C12 1.357(2) . ?
O1A C12A 1.236(2) . ?
O3A C12A 1.332(2) . ?
O2A C12A 1.281(2) . ?
O2 C12 1.264(2) . ?
O1 C12 1.237(2) . ?
N3 C4 1.333(2) . ?
N3 C3 1.460(2) . ?
N3 C5 1.464(2) . ?
N3A C4A 1.337(2) . ?
N3A C5A 1.457(2) . ?
N3A C3A 1.464(2) . ?
N2 C4 1.335(2) . ?
N2 C7 1.454(2) . ?
C4 N1 1.334(2) . ?
N1 C1 1.448(2) . ?
C4A N1A 1.327(2) . ?
C4A N2A 1.334(2) . ?
C5A C6A 1.524(3) . ?
N2A C7A 1.450(2) . ?
N1A C1A 1.446(2) . ?
C3 C2 1.524(2) . ?
C2 C1 1.521(2) . ?
C2 C9 1.532(3) . ?
C2 C8 1.535(2) . ?
C5 C6 1.520(3) . ?
C3A C2A 1.517(3) . ?
C7A C6A 1.519(3) . ?
C6A C10A 1.533(3) . ?
C6A C11A 1.537(2) . ?
C7 C6 1.526(3) . ?
C2A C8A 1.523(3) . ?
C2A C1A 1.526(3) . ?
C2A C9A 1.534(3) . ?
C6 C11 1.529(3) . ?
C6 C10 1.534(3) . ?
