#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/58/4075882.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_4075882
loop_
_publ_author_name
'Ison, Elon A.'
'Ortiz, Carlos O.'
'Abboud, Khalil'
'Boncella, James M.'
_publ_section_title
;
 Synthesis and Reactivity of Molybdenum(IV) Complexes with Alkyl and Aryl
 Isocyanides
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6310
_journal_paper_doi               10.1021/om0502436
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C39.5 H49 Mo N5 Si2'
_chemical_formula_weight         745.96
_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                102.802(2)
_cell_angle_beta                 93.928(2)
_cell_angle_gamma                94.868(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5484(9)
_cell_length_b                   11.8609(9)
_cell_length_c                   14.8731(12)
_cell_measurement_reflns_used    136
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1971.4(3)
_computing_cell_refinement       'Bruker SMART & SAINT (Bruker 1998)'
_computing_data_collection       'Bruker SMART (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'SMART CCD area detector'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12375
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9004
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, SHELXTL (Bruker 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0345P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                6271
_reflns_number_total             8614
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0502436si20050331_045034.cif
_cod_data_source_block           compound_2b
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C39.50 H49 Mo N5 Si2'
_cod_database_code               4075882
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
Mo Mo 0.644364(18) 1.634469(17) 0.744488(14) 0.02500(7) Uani 1 1 d . . .
Si1 Si 0.83243(6) 1.46523(6) 0.81843(4) 0.03051(16) Uani 1 1 d . . .
Si2 Si 0.67074(6) 1.92828(6) 0.79376(5) 0.02926(16) Uani 1 1 d . . .
N1 N 0.67434(16) 1.60949(16) 0.62865(12) 0.0273(4) Uani 1 1 d . . .
N2 N 0.77075(16) 1.59765(15) 0.83565(12) 0.0258(4) Uani 1 1 d . . .
N3 N 0.70884(15) 1.79994(15) 0.82258(12) 0.0252(4) Uani 1 1 d . . .
N4 N 0.50910(18) 1.38371(17) 0.74653(14) 0.0359(5) Uani 1 1 d . . .
N5 N 0.38559(18) 1.72204(17) 0.73548(13) 0.0319(5) Uani 1 1 d . . .
C1 C 0.7309(2) 1.59656(19) 0.54784(15) 0.0276(5) Uani 1 1 d . . .
C2 C 0.6684(2) 1.5638(2) 0.46107(16) 0.0352(6) Uani 1 1 d . . .
H2A H 0.5857 1.5503 0.4561 0.042 Uiso 1 1 calc R . .
C3 C 0.7277(3) 1.5508(2) 0.38199(18) 0.0463(7) Uani 1 1 d . . .
H3A H 0.6854 1.5287 0.3227 0.056 Uiso 1 1 calc R . .
C4 C 0.8468(3) 1.5697(3) 0.3890(2) 0.0558(8) Uani 1 1 d . . .
H4A H 0.8868 1.5609 0.3345 0.067 Uiso 1 1 calc R . .
C5 C 0.9085(3) 1.6011(3) 0.4736(2) 0.0655(10) Uani 1 1 d . . .
H5A H 0.9912 1.6137 0.4776 0.079 Uiso 1 1 calc R . .
C6 C 0.8518(2) 1.6149(3) 0.55359(19) 0.0498(8) Uani 1 1 d . . .
H6A H 0.8955 1.6368 0.6124 0.060 Uiso 1 1 calc R . .
C7 C 0.82252(19) 1.69379(19) 0.90591(15) 0.0250(5) Uani 1 1 d . . .
C8 C 0.79009(18) 1.80220(19) 0.89752(14) 0.0239(5) Uani 1 1 d . . .
C9 C 0.8366(2) 1.9003(2) 0.96533(15) 0.0291(5) Uani 1 1 d . . .
H9A H 0.8157 1.9747 0.9607 0.035 Uiso 1 1 calc R . .
C10 C 0.9125(2) 1.8912(2) 1.03898(16) 0.0310(5) Uani 1 1 d . . .
H10A H 0.9450 1.9593 1.0831 0.037 Uiso 1 1 calc R . .
C11 C 0.9410(2) 1.7839(2) 1.04845(16) 0.0325(6) Uani 1 1 d . . .
H11A H 0.9917 1.7773 1.0997 0.039 Uiso 1 1 calc R . .
C12 C 0.8951(2) 1.6855(2) 0.98263(16) 0.0305(5) Uani 1 1 d . . .
H12A H 0.9133 1.6112 0.9898 0.037 Uiso 1 1 calc R . .
C13 C 0.9958(2) 1.4883(2) 0.83528(17) 0.0414(6) Uani 1 1 d . . .
H13A H 1.0242 1.5452 0.8010 0.062 Uiso 1 1 calc R . .
H13B H 1.0279 1.4144 0.8123 0.062 Uiso 1 1 calc R . .
H13C H 1.0208 1.5172 0.9013 0.062 Uiso 1 1 calc R . .
C14 C 0.8032(2) 1.3781(2) 0.69598(18) 0.0480(7) Uani 1 1 d . . .
H14A H 0.7189 1.3581 0.6811 0.072 Uiso 1 1 calc R . .
H14B H 0.8420 1.3068 0.6891 0.072 Uiso 1 1 calc R . .
H14C H 0.8333 1.4241 0.6538 0.072 Uiso 1 1 calc R . .
C15 C 0.7757(2) 1.3767(2) 0.89849(19) 0.0445(7) Uani 1 1 d . . .
H15A H 0.7831 1.4247 0.9618 0.067 Uiso 1 1 calc R . .
H15B H 0.8209 1.3100 0.8963 0.067 Uiso 1 1 calc R . .
H15C H 0.6934 1.3490 0.8794 0.067 Uiso 1 1 calc R . .
C16 C 0.7988(2) 2.0399(2) 0.80320(18) 0.0422(7) Uani 1 1 d . . .
H16A H 0.8176 2.0807 0.8682 0.063 Uiso 1 1 calc R . .
H16B H 0.7796 2.0959 0.7664 0.063 Uiso 1 1 calc R . .
H16C H 0.8663 2.0015 0.7800 0.063 Uiso 1 1 calc R . .
C17 C 0.6146(2) 1.9016(2) 0.66908(16) 0.0403(6) Uani 1 1 d . . .
H17A H 0.6711 1.8621 0.6303 0.060 Uiso 1 1 calc R . .
H17B H 0.6035 1.9759 0.6530 0.060 Uiso 1 1 calc R . .
H17C H 0.5400 1.8527 0.6586 0.060 Uiso 1 1 calc R . .
C18 C 0.5617(2) 1.9945(2) 0.87012(19) 0.0484(7) Uani 1 1 d . . .
H18A H 0.4877 1.9444 0.8566 0.073 Uiso 1 1 calc R . .
H18B H 0.5494 2.0712 0.8590 0.073 Uiso 1 1 calc R . .
H18C H 0.5905 2.0028 0.9350 0.073 Uiso 1 1 calc R . .
C19 C 0.5577(2) 1.4727(2) 0.74480(16) 0.0338(6) Uani 1 1 d . . .
C20 C 0.4412(2) 1.2835(2) 0.75456(17) 0.0336(6) Uani 1 1 d . . .
C21 C 0.3890(2) 1.2864(2) 0.83673(19) 0.0418(7) Uani 1 1 d . . .
C22 C 0.3219(2) 1.1869(3) 0.8443(2) 0.0530(8) Uani 1 1 d . . .
H22A H 0.2870 1.1852 0.9000 0.064 Uiso 1 1 calc R . .
C23 C 0.3054(2) 1.0904(2) 0.7717(2) 0.0553(8) Uani 1 1 d . . .
H23A H 0.2581 1.0232 0.7774 0.066 Uiso 1 1 calc R . .
C24 C 0.3572(2) 1.0908(2) 0.6913(2) 0.0486(7) Uani 1 1 d . . .
H24A H 0.3442 1.0236 0.6419 0.058 Uiso 1 1 calc R . .
C25 C 0.4276(2) 1.1862(2) 0.67993(18) 0.0379(6) Uani 1 1 d . . .
C26 C 0.4790(2) 1.6920(2) 0.73789(15) 0.0289(5) Uani 1 1 d . . .
C27 C 0.2724(2) 1.75556(19) 0.73666(16) 0.0291(5) Uani 1 1 d . . .
C28 C 0.2211(2) 1.7691(2) 0.82069(18) 0.0389(6) Uani 1 1 d . . .
C29 C 0.1079(3) 1.8007(2) 0.8200(2) 0.0523(8) Uani 1 1 d . . .
H29A H 0.0693 1.8099 0.8752 0.063 Uiso 1 1 calc R . .
C30 C 0.0509(3) 1.8188(3) 0.7413(3) 0.0611(9) Uani 1 1 d . . .
H30A H -0.0265 1.8401 0.7428 0.073 Uiso 1 1 calc R . .
C31 C 0.1040(2) 1.8065(2) 0.6604(2) 0.0514(8) Uani 1 1 d . . .
H31A H 0.0634 1.8211 0.6071 0.062 Uiso 1 1 calc R . .
C32 C 0.2166(2) 1.7731(2) 0.65535(17) 0.0359(6) Uani 1 1 d . . .
C33 C 0.4069(3) 1.3921(3) 0.9151(2) 0.0684(10) Uani 1 1 d . . .
H33A H 0.3738 1.3737 0.9698 0.103 Uiso 1 1 calc R . .
H33B H 0.3679 1.4551 0.8973 0.103 Uiso 1 1 calc R . .
H33C H 0.4905 1.4165 0.9295 0.103 Uiso 1 1 calc R . .
C34 C 0.4859(3) 1.1865(2) 0.59275(19) 0.0586(8) Uani 1 1 d . . .
H34A H 0.4622 1.1131 0.5476 0.088 Uiso 1 1 calc R . .
H34B H 0.5708 1.1953 0.6068 0.088 Uiso 1 1 calc R . .
H34C H 0.4628 1.2513 0.5670 0.088 Uiso 1 1 calc R . .
C35 C 0.2850(3) 1.7488(3) 0.90516(19) 0.0628(9) Uani 1 1 d . . .
H35A H 0.2362 1.7641 0.9570 0.094 Uiso 1 1 calc R . .
H35B H 0.3575 1.8010 0.9203 0.094 Uiso 1 1 calc R . .
H35C H 0.3033 1.6680 0.8938 0.094 Uiso 1 1 calc R . .
C36 C 0.2736(3) 1.7553(2) 0.56674(17) 0.0488(7) Uani 1 1 d . . .
H36A H 0.3517 1.7979 0.5778 0.073 Uiso 1 1 calc R . .
H36B H 0.2265 1.7842 0.5210 0.073 Uiso 1 1 calc R . .
H36C H 0.2800 1.6723 0.5434 0.073 Uiso 1 1 calc R . .
C37 C 0.9795(4) 1.9187(4) 0.4183(3) 0.0846(12) Uani 1 1 d . . .
H37A H 0.9665 1.8630 0.3609 0.101 Uiso 0.50 1 calc PR A 1
C38 C 0.8949(4) 1.9295(4) 0.4789(3) 0.0937(14) Uani 1 1 d . . .
H38A H 0.8233 1.8810 0.4648 0.112 Uiso 1 1 calc R . .
C39 C 1.0843(4) 1.9893(5) 0.4409(3) 0.0926(13) Uani 1 1 d . . .
H39A H 1.1429 1.9802 0.3988 0.111 Uiso 1 1 calc R . .
C40 C 0.9534(6) 1.8431(6) 0.3351(5) 0.076(2) Uani 0.50 1 d P B 2
H40A H 1.0184 1.7960 0.3209 0.113 Uiso 0.50 1 calc PR B 2
H40B H 0.9401 1.8864 0.2870 0.113 Uiso 0.50 1 calc PR B 2
H40C H 0.8827 1.7921 0.3372 0.113 Uiso 0.50 1 calc PR B 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
N1 Mo N2 116.17(8) .
N1 Mo C26 101.59(9) .
N2 Mo C26 142.22(8) .
N1 Mo C19 99.56(9) .
N2 Mo C19 86.63(8) .
C26 Mo C19 86.05(9) .
N1 Mo N3 113.86(8) .
N2 Mo N3 77.61(7) .
C26 Mo N3 88.66(8) .
C19 Mo N3 146.55(8) .
N2 Si1 C15 110.34(10) .
N2 Si1 C13 111.58(11) .
C15 Si1 C13 109.97(13) .
N2 Si1 C14 112.44(11) .
C15 Si1 C14 109.24(13) .
C13 Si1 C14 103.03(12) .
N3 Si2 C18 110.54(11) .
N3 Si2 C17 111.28(10) .
C18 Si2 C17 110.82(13) .
N3 Si2 C16 113.09(11) .
C18 Si2 C16 108.04(13) .
C17 Si2 C16 102.80(12) .
C1 N1 Mo 163.59(16) .
C7 N2 Si1 119.67(15) .
C7 N2 Mo 115.68(14) .
Si1 N2 Mo 123.65(10) .
C8 N3 Si2 121.48(15) .
C8 N3 Mo 115.56(14) .
Si2 N3 Mo 122.88(10) .
C19 N4 C20 173.4(3) .
C26 N5 C27 176.9(2) .
C6 C1 N1 119.6(2) .
C6 C1 C2 119.3(2) .
N1 C1 C2 121.1(2) .
C3 C2 C1 119.6(2) .
C4 C3 C2 120.4(3) .
C5 C4 C3 120.4(3) .
C4 C5 C6 120.6(3) .
C5 C6 C1 119.8(3) .
C12 C7 C8 119.8(2) .
C12 C7 N2 124.9(2) .
C8 C7 N2 115.27(19) .
C7 C8 C9 118.1(2) .
C7 C8 N3 115.32(19) .
C9 C8 N3 126.5(2) .
C10 C9 C8 121.4(2) .
C11 C10 C9 120.1(2) .
C10 C11 C12 119.4(2) .
C11 C12 C7 121.1(2) .
N4 C19 Mo 178.8(2) .
C21 C20 N4 117.8(2) .
C21 C20 C25 123.2(2) .
N4 C20 C25 118.9(2) .
C22 C21 C20 117.5(2) .
C22 C21 C33 121.0(3) .
C20 C21 C33 121.4(2) .
C23 C22 C21 120.7(3) .
C24 C23 C22 120.3(3) .
C23 C24 C25 122.0(3) .
C24 C25 C20 116.2(2) .
C24 C25 C34 122.3(2) .
C20 C25 C34 121.5(2) .
N5 C26 Mo 178.2(2) .
C32 C27 N5 119.0(2) .
C32 C27 C28 123.6(2) .
N5 C27 C28 117.3(2) .
C29 C28 C27 116.4(3) .
C29 C28 C35 122.4(3) .
C27 C28 C35 121.2(2) .
C30 C29 C28 121.3(3) .
C29 C30 C31 121.0(3) .
C30 C31 C32 121.0(3) .
C31 C32 C27 116.7(2) .
C31 C32 C36 121.4(3) .
C27 C32 C36 121.9(2) .
C40 C37 C38 117.5(6) .
C40 C37 C39 122.5(6) .
C38 C37 C39 119.8(4) .
C39 C38 C37 118.5(4) 2_796
C38 C39 C37 121.7(4) 2_796
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo N1 1.7461(18) .
Mo N2 2.0637(19) .
Mo C26 2.085(3) .
Mo C19 2.088(3) .
Mo N3 2.0925(18) .
Si1 N2 1.7539(18) .
Si1 C15 1.869(2) .
Si1 C13 1.875(3) .
Si1 C14 1.876(3) .
Si2 N3 1.7526(19) .
Si2 C18 1.860(3) .
Si2 C17 1.871(2) .
Si2 C16 1.876(3) .
N1 C1 1.392(3) .
N2 C7 1.421(3) .
N3 C8 1.401(3) .
N4 C19 1.160(3) .
N4 C20 1.400(3) .
N5 C26 1.166(3) .
N5 C27 1.398(3) .
C1 C6 1.389(3) .
C1 C2 1.393(3) .
C2 C3 1.388(3) .
C3 C4 1.368(4) .
C4 C5 1.361(4) .
C5 C6 1.382(4) .
C7 C12 1.395(3) .
C7 C8 1.399(3) .
C8 C9 1.400(3) .
C9 C10 1.384(3) .
C10 C11 1.376(3) .
C11 C12 1.385(3) .
C20 C21 1.394(3) .
C20 C25 1.402(3) .
C21 C22 1.386(4) .
C21 C33 1.499(4) .
C22 C23 1.378(4) .
C23 C24 1.375(4) .
C24 C25 1.384(4) .
C25 C34 1.502(4) .
C27 C32 1.396(3) .
C27 C28 1.403(3) .
C28 C29 1.390(4) .
C28 C35 1.489(4) .
C29 C30 1.371(4) .
C30 C31 1.373(4) .
C31 C32 1.394(4) .
C32 C36 1.495(3) .
C37 C40 1.356(7) .
C37 C38 1.368(5) .
C37 C39 1.388(6) .
C38 C39 1.349(6) 2_796
C39 C38 1.349(6) 2_796
