#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/36/1513682.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_1513682
loop_
_publ_author_name
'Hering, Christian'
'Schulz, Axel'
'Villinger, Alexander'
_publ_section_title
;
 Diatomic PN -- trapped in a cyclo-tetraphosphazene
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              1064
_journal_paper_doi               10.1039/c3sc52322e
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C12 H15 Mo N3 O3'
_chemical_formula_sum            'C12 H15 Mo N3 O3'
_chemical_formula_weight         345.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 97.888(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.9362(2)
_cell_length_b                   13.8472(5)
_cell_length_c                   9.4000(3)
_cell_measurement_reflns_used    6097
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.072
_cell_measurement_theta_min      4.375
_cell_volume                     765.37(5)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14262
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.8601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0231
_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)+(0.0130P)²+0.1749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                2611
_reflns_number_total             2862
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3sc52322e.txt
_cod_data_source_block           ch157_[Mo(C2H5CN)3(CO)3]
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1513682
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Mo1 Mo 0.86420(2) 0.2500 -0.000358(14) 0.01484(4) Uani 1 2 d S
N1 N 0.6637(3) 0.2500 0.18221(16) 0.0242(3) Uani 1 2 d S
N2 N 0.60406(19) 0.14430(8) -0.09416(11) 0.0227(2) Uani 1 1 d .
O1 O 1.20381(18) 0.09652(8) 0.14196(11) 0.0340(2) Uani 1 1 d .
O2 O 1.1191(3) 0.2500 -0.26718(15) 0.0343(3) Uani 1 2 d S
C1 C 1.0749(2) 0.15392(10) 0.08731(13) 0.0227(2) Uani 1 1 d .
C2 C 1.0231(3) 0.2500 -0.16635(18) 0.0230(3) Uani 1 2 d S
C3 C 0.5591(3) 0.2500 0.27520(19) 0.0261(4) Uani 1 2 d S
C4 C 0.4326(5) 0.2411(16) 0.3978(2) 0.031(2) Uani 0.50 1 d P
H4A H 0.3547 0.1778 0.3936 0.038 Uiso 0.50 1 calc PR
H4B H 0.3148 0.2921 0.3919 0.038 Uiso 0.50 1 calc PR
C5 C 0.5882(4) 0.2500 0.5407(2) 0.0430(6) Uani 1 2 d S
H5A H 0.7025 0.1986 0.5481 0.064 Uiso 0.50 1 calc PR
H5B H 0.4976 0.2442 0.6199 0.064 Uiso 0.50 1 calc PR
H5C H 0.6642 0.3130 0.5457 0.064 Uiso 0.50 1 calc PR
C6 C 0.4644(2) 0.09131(9) -0.13817(13) 0.0228(2) Uani 1 1 d .
C7 C 0.2864(2) 0.02265(10) -0.19318(14) 0.0290(3) Uani 1 1 d .
H7A H 0.1389 0.0456 -0.1681 0.035 Uiso 1 1 calc R
H7B H 0.3197 -0.0406 -0.1459 0.035 Uiso 1 1 calc R
C8 C 0.2668(4) 0.00962(14) -0.35392(18) 0.0550(5) Uani 1 1 d .
H8A H 0.2219 0.0709 -0.4016 0.083 Uiso 1 1 calc R
H8B H 0.1517 -0.0396 -0.3847 0.083 Uiso 1 1 calc R
H8C H 0.4139 -0.0109 -0.3797 0.083 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'
Mo Mo -1.6832 0.6857 '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
C2 Mo1 C1 89.16(5) . 4_565
C2 Mo1 C1 89.16(5) . .
C1 Mo1 C1 87.08(7) 4_565 .
C2 Mo1 N1 176.84(6) . .
C1 Mo1 N1 93.13(5) 4_565 .
C1 Mo1 N1 93.13(5) . .
C2 Mo1 N2 93.97(5) . .
C1 Mo1 N2 176.18(5) 4_565 .
C1 Mo1 N2 95.14(5) . .
N1 Mo1 N2 83.66(4) . .
C2 Mo1 N2 93.97(5) . 4_565
C1 Mo1 N2 95.14(5) 4_565 4_565
C1 Mo1 N2 176.18(5) . 4_565
N1 Mo1 N2 83.66(4) . 4_565
N2 Mo1 N2 82.47(5) . 4_565
C3 N1 Mo1 179.43(15) . .
C6 N2 Mo1 177.01(11) . .
O1 C1 Mo1 179.07(11) . .
O2 C2 Mo1 179.91(16) . .
N1 C3 C4 174.8(8) . 4_565
N1 C3 C4 174.8(8) . .
C4 C3 C4 9.6(17) 4_565 .
C3 C4 C5 111.8(3) . .
C3 C4 H4A 109.3 . .
C5 C4 H4A 109.3 . .
C3 C4 H4B 109.3 . .
C5 C4 H4B 109.3 . .
H4A C4 H4B 107.9 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 C7 179.32(14) . .
C6 C7 C8 112.61(13) . .
C6 C7 H7A 109.1 . .
C8 C7 H7A 109.1 . .
C6 C7 H7B 109.1 . .
C8 C7 H7B 109.1 . .
H7A C7 H7B 107.8 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C2 1.9307(19) .
Mo1 C1 1.9315(13) 4_565
Mo1 C1 1.9315(13) .
Mo1 N1 2.2185(16) .
Mo1 N2 2.2206(11) .
Mo1 N2 2.2205(11) 4_565
N1 C3 1.140(2) .
N2 C6 1.1414(16) .
O1 C1 1.1719(16) .
O2 C2 1.171(2) .
C3 C4 1.465(4) 4_565
C3 C4 1.465(4) .
C4 C5 1.526(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.4620(18) .
C7 C8 1.510(2) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 Mo1 N1 C3 0.00(2) . .
C1 Mo1 N1 C3 136.38(4) 4_565 .
C1 Mo1 N1 C3 -136.38(4) . .
N2 Mo1 N1 C3 -41.54(4) . .
N2 Mo1 N1 C3 41.55(4) 4_565 .
C2 Mo1 N2 C6 -160.3(19) . .
C1 Mo1 N2 C6 -15(2) 4_565 .
C1 Mo1 N2 C6 110.2(19) . .
N1 Mo1 N2 C6 17.6(19) . .
N2 Mo1 N2 C6 -66.8(19) 4_565 .
C2 Mo1 C1 O1 115(8) . .
C1 Mo1 C1 O1 26(8) 4_565 .
N1 Mo1 C1 O1 -67(8) . .
N2 Mo1 C1 O1 -151(8) . .
N2 Mo1 C1 O1 -99(8) 4_565 .
C1 Mo1 C2 O2 -136.5(3) 4_565 .
C1 Mo1 C2 O2 136.5(3) . .
N1 Mo1 C2 O2 0.0(3) . .
N2 Mo1 C2 O2 41.4(3) . .
N2 Mo1 C2 O2 -41.4(3) 4_565 .
Mo1 N1 C3 C4 -113(4) . 4_565
Mo1 N1 C3 C4 113(4) . .
N1 C3 C4 C5 74(5) . .
C4 C3 C4 C5 -83.1(12) 4_565 .
Mo1 N2 C6 C7 -83(14) . .
N2 C6 C7 C8 -134(14) . .
