#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179333 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/30/4323058.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_4323058
loop_
_publ_author_name
'Myra B. O'Donoghue'
'William M. Davis'
'Richard R. Schrock'
_publ_section_title
;
 Derivatization of Dinitrogen by Molybdenum in Triamidoamine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5149
_journal_page_last               5158
_journal_paper_doi               10.1021/ic9803513
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C18 H49 Mo N6 Si3'
_chemical_formula_weight         529.84
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.80(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.235(3)
_cell_length_b                   14.315(7)
_cell_length_c                   20.277(7)
_cell_measurement_temperature    183(2)
_cell_volume                     2885.1(19)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11505
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.024
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.024
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_obs          0.0251
_refine_ls_shift/esd_max         0.023
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+2.4973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0750
_refine_ls_wR_factor_obs         0.0705
_reflns_number_observed          3960
_reflns_number_total             4130
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9803513_5.cif
_cod_data_source_block           C18H49MoN6Si3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+2.4973P] 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^)+(0.0354P)^2^+2.4973P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323058
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.29233(2) 0.963944(14) 0.146394(9) 0.02750(10) Uani 1 d . 1
Si1 Si 0.61101(7) 0.95090(5) 0.14086(4) 0.0347(2) Uani 1 d . 1
Si2 Si 0.35381(8) 0.66228(5) 0.11298(4) 0.0415(2) Uani 1 d . 1
Si3 Si 0.18629(7) 0.88950(5) 0.27779(3) 0.0377(2) Uani 1 d . 1
N1 N 0.4727(2) 1.01714(14) 0.14978(10) 0.0308(4) Uani 1 d . 1
N2 N 0.0988(5) 1.3046(3) 0.0048(2) 0.0469(11) Uani 0.50 d P 1
N3 N 0.1964(2) 0.97816(14) 0.21986(10) 0.0353(5) Uani 1 d . 1
N4 N 0.2406(2) 1.12134(14) 0.13621(10) 0.0310(4) Uani 1 d . 1
N5 N 0.3382(2) 0.84327(14) 0.15674(9) 0.0297(4) Uani 1 d . 1
N6 N 0.3689(2) 0.76020(15) 0.16387(10) 0.0392(5) Uani 1 d . 1
H6A H 0.4092(2) 0.74720(15) 0.20625(10) 0.047 Uiso 1 calc R 1
C1 C 0.4862(2) 1.1199(2) 0.15480(13) 0.0351(6) Uani 1 d . 1
H1A H 0.4878(2) 1.1464(2) 0.10991(13) 0.042 Uiso 1 calc R 1
H1B H 0.5715(2) 1.1367(2) 0.18731(13) 0.042 Uiso 1 calc R 1
C2 C 0.3685(2) 1.1596(2) 0.17867(12) 0.0348(5) Uani 1 d . 1
H2A H 0.3767(2) 1.1430(2) 0.22687(12) 0.042 Uiso 1 calc R 1
H2B H 0.3683(2) 1.2286(2) 0.17501(12) 0.042 Uiso 1 calc R 1
C3 C 0.1954(3) 1.2682(2) 0.06293(14) 0.0498(7) Uani 1 d . 1
H3A H 0.1703(3) 1.2904(2) 0.10450(14) 0.060 Uiso 1 calc R 1
H3B H 0.2846(3) 1.2951(2) 0.06312(14) 0.060 Uiso 1 calc R 1
C4 C 0.2088(3) 1.1619(2) 0.06675(12) 0.0396(6) Uani 1 d . 1
H4A H 0.1235(3) 1.1342(2) 0.04069(12) 0.048 Uiso 1 calc R 1
H4B H 0.2804(3) 1.1431(2) 0.04408(12) 0.048 Uiso 1 calc R 1
C5 C 0.1450(3) 1.0720(2) 0.23115(13) 0.0407(6) Uani 1 d . 1
H5A H 0.2090(3) 1.1027(2) 0.26935(13) 0.049 Uiso 1 calc R 1
H5B H 0.0578(3) 1.0655(2) 0.24382(13) 0.049 Uiso 1 calc R 1
C6 C 0.1262(3) 1.1327(2) 0.16850(14) 0.0421(6) Uani 1 d . 1
H6B H 0.0415(3) 1.1153(2) 0.13574(14) 0.051 Uiso 1 calc R 1
H6C H 0.1193(3) 1.1990(2) 0.18122(14) 0.051 Uiso 1 calc R 1
C7 C 0.1634(3) 0.9382(2) 0.04752(14) 0.0466(7) Uani 1 d . 1
H7A H 0.1217(3) 0.9970(2) 0.02842(14) 0.070 Uiso 1 calc R 1
H7B H 0.0931(3) 0.8936(2) 0.05153(14) 0.070 Uiso 1 calc R 1
H7C H 0.2166(3) 0.9124(2) 0.01759(14) 0.070 Uiso 1 calc R 1
C11 C 0.5641(3) 0.8845(2) 0.05931(14) 0.0488(7) Uani 1 d . 1
H11A H 0.5333(3) 0.9281(2) 0.02157(14) 0.073 Uiso 1 calc R 1
H11B H 0.4918(3) 0.8404(2) 0.06101(14) 0.073 Uiso 1 calc R 1
H11C H 0.6427(3) 0.8500(2) 0.05257(14) 0.073 Uiso 1 calc R 1
C12 C 0.6696(3) 0.8684(2) 0.21287(15) 0.0474(7) Uani 1 d . 1
H12A H 0.6941(3) 0.9036(2) 0.25553(15) 0.071 Uiso 1 calc R 1
H12B H 0.7483(3) 0.8340(2) 0.20628(15) 0.071 Uiso 1 calc R 1
H12C H 0.5973(3) 0.8243(2) 0.21471(15) 0.071 Uiso 1 calc R 1
C13 C 0.7549(3) 1.0304(2) 0.1375(2) 0.0552(8) Uani 1 d . 1
H13A H 0.7267(3) 1.0747(2) 0.1000(2) 0.083 Uiso 1 calc R 1
H13B H 0.8308(3) 0.9933(2) 0.1305(2) 0.083 Uiso 1 calc R 1
H13C H 0.7822(3) 1.0648(2) 0.1804(2) 0.083 Uiso 1 calc R 1
C21 C 0.2657(5) 0.5731(3) 0.1531(2) 0.094(2) Uani 1 d . 1
H21A H 0.3164(5) 0.5623(3) 0.2000(2) 0.142 Uiso 1 calc R 1
H21B H 0.2593(5) 0.5145(3) 0.1275(2) 0.142 Uiso 1 calc R 1
H21C H 0.1752(5) 0.5953(3) 0.1531(2) 0.142 Uiso 1 calc R 1
C22 C 0.2619(3) 0.6852(2) 0.02409(14) 0.0568(8) Uani 1 d . 1
H22A H 0.1713(3) 0.7080(2) 0.02332(14) 0.085 Uiso 1 calc R 1
H22B H 0.2556(3) 0.6273(2) -0.00229(14) 0.085 Uiso 1 calc R 1
H22C H 0.3104(3) 0.7324(2) 0.00421(14) 0.085 Uiso 1 calc R 1
C23 C 0.5247(4) 0.6193(3) 0.1128(2) 0.0808(12) Uani 1 d . 1
H23A H 0.5747(4) 0.6069(3) 0.1595(2) 0.121 Uiso 1 calc R 1
H23B H 0.5722(4) 0.6668(3) 0.0926(2) 0.121 Uiso 1 calc R 1
H23C H 0.5175(4) 0.5617(3) 0.0861(2) 0.121 Uiso 1 calc R 1
C31 C 0.0876(4) 0.9315(3) 0.3389(2) 0.0627(9) Uani 1 d . 1
H31A H -0.0026(4) 0.9502(3) 0.3138(2) 0.094 Uiso 1 calc R 1
H31B H 0.1335(4) 0.9851(3) 0.3644(2) 0.094 Uiso 1 calc R 1
H31C H 0.0805(4) 0.8811(3) 0.3706(2) 0.094 Uiso 1 calc R 1
C32 C 0.0954(3) 0.7863(2) 0.2335(2) 0.0626(9) Uani 1 d . 1
H32A H 0.0056(3) 0.8053(2) 0.2078(2) 0.094 Uiso 1 calc R 1
H32B H 0.0869(3) 0.7388(2) 0.2670(2) 0.094 Uiso 1 calc R 1
H32C H 0.1457(3) 0.7604(2) 0.2022(2) 0.094 Uiso 1 calc R 1
C33 C 0.3567(3) 0.8545(2) 0.32652(15) 0.0529(7) Uani 1 d . 1
H33A H 0.4040(3) 0.9092(2) 0.34972(15) 0.079 Uiso 1 calc R 1
H33B H 0.4074(3) 0.8287(2) 0.29538(15) 0.079 Uiso 1 calc R 1
H33C H 0.3486(3) 0.8070(2) 0.36018(15) 0.079 Uiso 1 calc R 1
C212 C 0.0934(7) 1.4062(4) 0.0066(3) 0.056(2) Uani 0.50 d P 1
H21D H 0.0272(7) 1.4290(4) -0.0334(3) 0.084 Uiso 0.50 calc PR 1
H21E H 0.1822(7) 1.4319(4) 0.0066(3) 0.084 Uiso 0.50 calc PR 1
H21F H 0.0672(7) 1.4262(4) 0.0479(3) 0.084 Uiso 0.50 calc PR 1
C213 C 0.1226(4) 1.2735(3) -0.0593(2) 0.0663(9) Uani 1 d . 1
H21G H 0.0543(4) 1.3004(3) -0.0968(2) 0.099 Uiso 1 calc R 1
H21H H 0.1175(4) 1.2052(3) -0.0618(2) 0.099 Uiso 1 calc R 1
H21I H 0.2121(4) 1.2939(3) -0.0628(2) 0.099 Uiso 1 calc R 1
N2' N 0.2197(5) 1.3031(3) -0.0010(2) 0.0417(11) Uani 0.50 d P 2
C211 C 0.2300(10) 1.4045(5) 0.0010(4) 0.084(3) Uani 0.50 d P 2
H21J H 0.1508(31) 1.4309(5) 0.0135(31) 0.125 Uiso 0.50 calc PR 2
H21K H 0.2347(65) 1.4279(6) -0.0437(9) 0.125 Uiso 0.50 calc PR 2
H21L H 0.3114(34) 1.4230(5) 0.0348(23) 0.125 Uiso 0.50 calc PR 2
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'
Si Si 0.0817 0.0704 '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
N5 Mo1 N3 100.05(8) . . ?
N5 Mo1 N1 98.65(8) . . ?
N3 Mo1 N1 123.99(9) . . ?
N5 Mo1 C7 91.69(10) . . ?
N3 Mo1 C7 114.47(11) . . ?
N1 Mo1 C7 117.18(10) . . ?
N5 Mo1 N4 177.74(8) . . ?
N3 Mo1 N4 79.81(8) . . ?
N1 Mo1 N4 79.63(8) . . ?
C7 Mo1 N4 90.42(9) . . ?
N1 Si1 C12 112.32(12) . . ?
N1 Si1 C11 108.92(12) . . ?
C12 Si1 C11 109.75(14) . . ?
N1 Si1 C13 109.68(12) . . ?
C12 Si1 C13 107.71(14) . . ?
C11 Si1 C13 108.38(15) . . ?
N6 Si2 C22 112.96(13) . . ?
N6 Si2 C23 108.71(14) . . ?
C22 Si2 C23 108.5(2) . . ?
N6 Si2 C21 106.24(15) . . ?
C22 Si2 C21 111.2(2) . . ?
C23 Si2 C21 109.2(2) . . ?
N3 Si3 C33 110.79(13) . . ?
N3 Si3 C32 110.79(14) . . ?
C33 Si3 C32 109.9(2) . . ?
N3 Si3 C31 109.79(13) . . ?
C33 Si3 C31 108.69(15) . . ?
C32 Si3 C31 106.7(2) . . ?
C1 N1 Si1 118.8(2) . . ?
C1 N1 Mo1 117.11(15) . . ?
Si1 N1 Mo1 123.93(11) . . ?
C3 N2 C213 113.2(4) . . ?
C3 N2 C212 111.2(4) . . ?
C213 N2 C212 110.2(4) . . ?
C5 N3 Si3 118.3(2) . . ?
C5 N3 Mo1 117.9(2) . . ?
Si3 N3 Mo1 123.36(11) . . ?
C6 N4 C4 111.0(2) . . ?
C6 N4 C2 112.5(2) . . ?
C4 N4 C2 111.6(2) . . ?
C6 N4 Mo1 104.82(15) . . ?
C4 N4 Mo1 117.34(14) . . ?
C2 N4 Mo1 99.01(14) . . ?
N6 N5 Mo1 179.5(2) . . ?
N5 N6 Si2 137.0(2) . . ?
N1 C1 C2 109.1(2) . . ?
N4 C2 C1 109.5(2) . . ?
N2 C3 C4 115.9(3) . . ?
N4 C4 C3 115.7(2) . . ?
N3 C5 C6 111.7(2) . . ?
N4 C6 C5 110.6(2) . . ?
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 N5 1.789(2) . ?
Mo1 N3 1.981(2) . ?
Mo1 N1 1.983(2) . ?
Mo1 C7 2.153(3) . ?
Mo1 N4 2.312(2) . ?
Si1 N1 1.749(2) . ?
Si1 C12 1.862(3) . ?
Si1 C11 1.868(3) . ?
Si1 C13 1.875(3) . ?
Si2 N6 1.726(2) . ?
Si2 C22 1.852(3) . ?
Si2 C23 1.855(4) . ?
Si2 C21 1.859(4) . ?
Si3 N3 1.749(2) . ?
Si3 C33 1.856(3) . ?
Si3 C32 1.859(3) . ?
Si3 C31 1.875(3) . ?
N1 C1 1.479(3) . ?
N2 C3 1.443(5) . ?
N2 C213 1.448(6) . ?
N2 C212 1.456(7) . ?
N3 C5 1.480(3) . ?
N4 C6 1.481(3) . ?
N4 C4 1.486(3) . ?
N4 C2 1.489(3) . ?
N5 N6 1.229(3) . ?
C1 C2 1.512(3) . ?
C3 C4 1.528(4) . ?
C5 C6 1.513(4) . ?
N2' C211 1.456(8) . ?
