#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/84/1508405.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_1508405
loop_
_publ_author_name
'Budge, Matthew G.'
'Muir, Kathleen J.'
'McQuillan, Geoffrey P.'
'Harrison, William T.A.'
_publ_section_title
;
 Short Intramolecular N-H...C(carbonyl) Interactions in Mixed-Ligand
 Molybdenum Hexacarbonyl Derivatives
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              47
_journal_page_last               58
_journal_paper_doi               10.3390/cryst1020047
_journal_volume                  1
_journal_year                    2012
_chemical_formula_moiety         'C24 H19 Mo N5 O3'
_chemical_formula_sum            'C24 H19 Mo N5 O3'
_chemical_formula_weight         521.38
_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   'difmap (N-H) and geom (C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.065(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4222(3)
_cell_length_b                   21.5966(9)
_cell_length_c                   12.5011(5)
_cell_measurement_reflns_used    6705
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.49
_cell_volume                     2268.12(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       ω
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13657
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0398P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                3269
_reflns_number_total             3998
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file
C24H19MoN5O3_P21_n_crystals-01-00047-s001_moco3_DC150.CIF
_cod_data_source_block           gm005_chateigner_1508405
_cod_depositor_comments          'journal volume and issue reversed'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1508405
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 0.05620(2) 0.356529(9) 0.720913(14) 0.04382(8) Uani 1 1 d .
C1 C 0.1443(3) 0.32525(11) 0.59322(18) 0.0512(5) Uani 1 1 d .
C2 C 0.1654(3) 0.28627(11) 0.78913(16) 0.0498(5) Uani 1 1 d .
C3 C 0.2547(3) 0.40227(12) 0.73790(18) 0.0574(6) Uani 1 1 d .
O1 O 0.2048(2) 0.30660(9) 0.51843(13) 0.0717(5) Uani 1 1 d .
O2 O 0.2360(2) 0.24376(8) 0.82608(14) 0.0693(5) Uani 1 1 d .
O3 O 0.3766(3) 0.42872(10) 0.74376(18) 0.0914(6) Uani 1 1 d .
N1 N -0.0851(2) 0.43398(9) 0.63253(13) 0.0477(4) Uani 1 1 d .
N2 N -0.1834(2) 0.30772(9) 0.69577(14) 0.0478(4) Uani 1 1 d .
N3 N -0.0590(2) 0.39726(9) 0.87371(13) 0.0481(4) Uani 1 1 d .
N4 N 0.1708(3) 0.37820(11) 0.97805(16) 0.0598(6) Uani 1 1 d .
H4 H 0.200(4) 0.3619(12) 0.927(2) 0.072 Uiso 1 1 d .
N5 N 0.2803(3) 0.40839(11) 1.14732(16) 0.0693(6) Uani 1 1 d .
C4 C -0.0552(3) 0.49321(11) 0.65850(19) 0.0561(6) Uani 1 1 d .
H4A H 0.0210 0.5015 0.7141 0.067 Uiso 1 1 calc R
C5 C -0.1313(3) 0.54243(12) 0.6073(2) 0.0656(7) Uani 1 1 d .
H5 H -0.1064 0.5829 0.6278 0.079 Uiso 1 1 calc R
C6 C -0.2441(3) 0.53094(14) 0.5258(2) 0.0710(8) Uani 1 1 d .
H6 H -0.2971 0.5633 0.4896 0.085 Uiso 1 1 calc R
C7 C -0.2777(3) 0.47047(13) 0.49848(19) 0.0628(7) Uani 1 1 d .
H7 H -0.3553 0.4616 0.4440 0.075 Uiso 1 1 calc R
C8 C -0.1960(3) 0.42254(11) 0.55200(16) 0.0492(5) Uani 1 1 d .
C9 C -0.2241(3) 0.35611(11) 0.51936(17) 0.0548(6) Uani 1 1 d .
H9A H -0.3030 0.3553 0.4590 0.066 Uiso 1 1 calc R
H9B H -0.1259 0.3396 0.4949 0.066 Uiso 1 1 calc R
C10 C -0.2786(3) 0.31434(11) 0.60443(17) 0.0499(5) Uani 1 1 d .
C11 C -0.4208(3) 0.28247(13) 0.5898(2) 0.0642(7) Uani 1 1 d .
H11 H -0.4843 0.2873 0.5263 0.077 Uiso 1 1 calc R
C12 C -0.4689(3) 0.24381(14) 0.6682(2) 0.0752(8) Uani 1 1 d .
H12 H -0.5643 0.2222 0.6583 0.090 Uiso 1 1 calc R
C13 C -0.3739(3) 0.23747(13) 0.7618(2) 0.0695(7) Uani 1 1 d .
H13 H -0.4039 0.2120 0.8169 0.083 Uiso 1 1 calc R
C14 C -0.2335(3) 0.26987(11) 0.77136(19) 0.0583(6) Uani 1 1 d .
H14 H -0.1689 0.2653 0.8343 0.070 Uiso 1 1 calc R
C15 C -0.2097(3) 0.41841(11) 0.86440(19) 0.0560(6) Uani 1 1 d .
H15 H -0.2664 0.4140 0.7982 0.067 Uiso 1 1 calc R
C16 C -0.2855(3) 0.44583(12) 0.9451(2) 0.0622(6) Uani 1 1 d .
H16 H -0.3895 0.4601 0.9339 0.075 Uiso 1 1 calc R
C17 C -0.2023(3) 0.45165(12) 1.0439(2) 0.0665(7) Uani 1 1 d .
H17 H -0.2500 0.4704 1.1005 0.080 Uiso 1 1 calc R
C18 C -0.0501(3) 0.42989(12) 1.05846(19) 0.0600(6) Uani 1 1 d .
H18 H 0.0063 0.4332 1.1249 0.072 Uiso 1 1 calc R
C19 C 0.0195(3) 0.40260(11) 0.97222(17) 0.0492(5) Uani 1 1 d .
C20 C 0.2909(3) 0.37550(11) 1.05923(17) 0.0504(6) Uani 1 1 d .
C21 C 0.4219(3) 0.33836(12) 1.0416(2) 0.0605(6) Uani 1 1 d .
H21 H 0.4243 0.3153 0.9789 0.073 Uiso 1 1 calc R
C22 C 0.5460(3) 0.33636(13) 1.1173(2) 0.0675(7) Uani 1 1 d .
H22 H 0.6341 0.3116 1.1072 0.081 Uiso 1 1 calc R
C23 C 0.5400(4) 0.37108(16) 1.2083(2) 0.0776(9) Uani 1 1 d .
H23 H 0.6241 0.3711 1.2607 0.093 Uiso 1 1 calc R
C24 C 0.4075(4) 0.40556(16) 1.2197(2) 0.0832(9) Uani 1 1 d .
H24 H 0.4038 0.4290 1.2819 0.100 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
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C1 Mo1 C2 83.78(9) y
C1 Mo1 C3 83.69(10) y
C2 Mo1 C3 88.41(10) y
C1 Mo1 N2 96.47(8) y
C2 Mo1 N2 94.96(8) y
C3 Mo1 N2 176.63(8) y
C1 Mo1 N1 94.22(8) y
C2 Mo1 N1 175.45(8) y
C3 Mo1 N1 95.45(8) y
N2 Mo1 N1 81.18(7) y
C1 Mo1 N3 177.83(8) y
C2 Mo1 N3 98.30(8) y
C3 Mo1 N3 96.97(8) y
N2 Mo1 N3 82.75(6) y
N1 Mo1 N3 83.66(6) y
O1 C1 Mo1 176.8(2) ?
O2 C2 Mo1 176.7(2) ?
O3 C3 Mo1 176.9(2) ?
C4 N1 C8 117.7(2) ?
C4 N1 Mo1 119.90(15) ?
C8 N1 Mo1 122.38(15) ?
C14 N2 C10 117.5(2) ?
C14 N2 Mo1 120.33(14) ?
C10 N2 Mo1 122.18(15) ?
C15 N3 C19 116.35(19) ?
C15 N3 Mo1 119.55(14) ?
C19 N3 Mo1 124.07(14) ?
C19 N4 C20 133.0(2) ?
C19 N4 H4 118(2) ?
C20 N4 H4 109(2) ?
C20 N5 C24 115.9(2) ?
N1 C4 C5 123.5(2) ?
N1 C4 H4A 118.2 ?
C5 C4 H4A 118.2 ?
C6 C5 C4 118.9(3) ?
C6 C5 H5 120.6 ?
C4 C5 H5 120.6 ?
C5 C6 C7 118.6(2) ?
C5 C6 H6 120.7 ?
C7 C6 H6 120.7 ?
C6 C7 C8 120.2(2) ?
C6 C7 H7 119.9 ?
C8 C7 H7 119.9 ?
N1 C8 C7 121.1(2) ?
N1 C8 C9 117.70(19) ?
C7 C8 C9 121.1(2) ?
C10 C9 C8 115.69(18) ?
C10 C9 H9A 108.4 ?
C8 C9 H9A 108.4 ?
C10 C9 H9B 108.4 ?
C8 C9 H9B 108.4 ?
H9A C9 H9B 107.4 ?
N2 C10 C11 121.0(2) ?
N2 C10 C9 118.1(2) ?
C11 C10 C9 120.9(2) ?
C12 C11 C10 120.3(2) ?
C12 C11 H11 119.8 ?
C10 C11 H11 119.8 ?
C11 C12 C13 119.1(2) ?
C11 C12 H12 120.5 ?
C13 C12 H12 120.5 ?
C14 C13 C12 117.9(2) ?
C14 C13 H13 121.0 ?
C12 C13 H13 121.0 ?
N2 C14 C13 124.2(2) ?
N2 C14 H14 117.9 ?
C13 C14 H14 117.9 ?
N3 C15 C16 124.8(2) ?
N3 C15 H15 117.6 ?
C16 C15 H15 117.6 ?
C15 C16 C17 117.8(2) ?
C15 C16 H16 121.1 ?
C17 C16 H16 121.1 ?
C18 C17 C16 119.9(2) ?
C18 C17 H17 120.0 ?
C16 C17 H17 120.0 ?
C17 C18 C19 119.0(2) ?
C17 C18 H18 120.5 ?
C19 C18 H18 120.5 ?
N3 C19 N4 113.83(19) ?
N3 C19 C18 122.1(2) ?
N4 C19 C18 124.0(2) ?
N5 C20 N4 120.1(2) ?
N5 C20 C21 122.9(2) ?
N4 C20 C21 117.0(2) ?
C22 C21 C20 119.1(2) ?
C22 C21 H21 120.5 ?
C20 C21 H21 120.5 ?
C21 C22 C23 119.3(3) ?
C21 C22 H22 120.3 ?
C23 C22 H22 120.3 ?
C24 C23 C22 117.9(3) ?
C24 C23 H23 121.0 ?
C22 C23 H23 121.0 ?
N5 C24 C23 124.9(3) ?
N5 C24 H24 117.6 ?
C23 C24 H24 117.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 C1 1.929(3) y
Mo1 C2 1.940(2) y
Mo1 C3 1.940(3) y
Mo1 N2 2.2788(18) y
Mo1 N1 2.2908(18) y
Mo1 N3 2.3719(18) y
C1 O1 1.168(3) y
C2 O2 1.171(3) y
C3 O3 1.173(3) y
N1 C4 1.339(3) ?
N1 C8 1.347(3) ?
N2 C14 1.340(3) ?
N2 C10 1.355(3) ?
N3 C15 1.347(3) ?
N3 C19 1.361(3) ?
N4 C19 1.376(3) ?
N4 C20 1.382(3) ?
N4 H4 0.78(3) ?
N5 C20 1.319(3) ?
N5 C24 1.354(3) ?
C4 C5 1.376(3) ?
C4 H4A 0.9300 ?
C5 C6 1.365(4) ?
C5 H5 0.9300 ?
C6 C7 1.374(4) ?
C6 H6 0.9300 ?
C7 C8 1.388(3) ?
C7 H7 0.9300 ?
C8 C9 1.505(3) ?
C9 C10 1.492(3) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 C11 1.383(3) ?
C11 C12 1.371(4) ?
C11 H11 0.9300 ?
C12 C13 1.377(4) ?
C12 H12 0.9300 ?
C13 C14 1.372(3) ?
C13 H13 0.9300 ?
C14 H14 0.9300 ?
C15 C16 1.367(3) ?
C15 H15 0.9300 ?
C16 C17 1.382(4) ?
C16 H16 0.9300 ?
C17 C18 1.366(4) ?
C17 H17 0.9300 ?
C18 C19 1.394(3) ?
C18 H18 0.9300 ?
C20 C21 1.394(4) ?
C21 C22 1.360(3) ?
C21 H21 0.9300 ?
C22 C23 1.366(4) ?
C22 H22 0.9300 ?
C23 C24 1.358(4) ?
C23 H23 0.9300 ?
C24 H24 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N4 H4 C2 0.78(3) 2.38(3) 3.083(3) 151(3)
N4 H4 C3 0.78(3) 2.59(3) 3.175(3) 133(2)
C18 H18 N5 0.93 2.37 2.959(3) 121
