#------------------------------------------------------------------------------
#$Date: 2015-08-05 17:32:54 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152772 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/61/4086148.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_4086148
loop_
_publ_author_name
'Ohki, Yasuhiro'
'Aoyagi, Keiya'
'Seino, Hidetake'
_publ_section_title
;
 Synthesis and Protonation of N-Heterocyclic-Carbene-Supported Dinitrogen
 Complexes of Molybdenum(0)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3414
_journal_paper_doi               10.1021/acs.organomet.5b00391
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C28 H48 Mo N12'
_chemical_formula_sum            'C28 H48 Mo N12'
_chemical_formula_weight         648.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   12.113(6)
_cell_length_b                   12.113(6)
_cell_length_c                   11.029(6)
_cell_measurement_reflns_used    4692
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.40
_cell_volume                     1618.2(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_laue_measured_fraction_full 0.000
_diffrn_reflns_laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5928
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.470
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         3.364
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  767 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1749
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0000P)²+0.8458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                1533
_reflns_number_total             1749
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om5b00391_si_002.cif
_cod_data_source_block           aoyagi17
_cod_database_code               4086148
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -Y,+X,+Z
3 -X,-Y,+Z
4 +Y,-X,+Z
5 1/2-X,1/2+Y,1/2+Z
6 1/2+Y,1/2+X,1/2+Z
7 1/2+X,1/2-Y,1/2+Z
8 1/2-Y,1/2-X,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_site_symmetry_multiplicity
_atom_site_calc_flag
Mo1 Mo 0.5 0.5 0.61479(8) 0.01485(8) Uani 1 2 d
N1 N 0.5 0.5 0.7940(8) 0.016(2) Uani 1 2 d
N2 N 0.5 0.5 0.8969(9) 0.028(3) Uani 1 2 d
N3 N 0.5 0.5 0.4335(10) 0.023(3) Uani 1 2 d
N4 N 0.5 0.5 0.3302(9) 0.037(3) Uani 1 2 d
N5 N 0.5846(3) 0.74252(19) 0.7047(3) 0.0179(7) Uani 1 8 d
N6 N 0.6918(2) 0.6839(2) 0.5644(2) 0.0189(7) Uani 1 8 d
C1 C 0.5953(3) 0.6559(2) 0.6244(4) 0.0163(7) Uani 1 8 d
C2 C 0.6717(3) 0.8184(3) 0.6963(4) 0.0218(9) Uani 1 8 d
C3 C 0.7394(2) 0.7812(2) 0.6097(5) 0.0215(7) Uani 1 8 d
C4 C 0.4912(3) 0.7617(3) 0.7836(3) 0.0246(9) Uani 1 8 d
C5 C 0.7422(3) 0.6175(3) 0.4701(4) 0.0243(9) Uani 1 8 d
C6 C 0.6807(3) 0.9167(3) 0.7770(4) 0.0348(13) Uani 1 8 d
C7 C 0.8469(3) 0.8238(3) 0.5637(4) 0.0325(11) Uani 1 8 d
H4A H 0.4432 0.6966 0.7833 0.0295 Uiso 1 8 calc
H4B H 0.4497 0.8259 0.7547 0.0295 Uiso 1 8 calc
H4C H 0.5175 0.7755 0.8662 0.0295 Uiso 1 8 calc
H5A H 0.8129 0.5884 0.4992 0.0293 Uiso 1 8 calc
H5B H 0.7547 0.6631 0.3981 0.0293 Uiso 1 8 calc
H5C H 0.6931 0.556 0.4494 0.0293 Uiso 1 8 calc
H6A H 0.6206 0.9682 0.7591 0.0419 Uiso 1 8 calc
H6B H 0.7518 0.9533 0.7632 0.0419 Uiso 1 8 calc
H6C H 0.6759 0.8932 0.8619 0.0419 Uiso 1 8 calc
H7A H 0.8692 0.8881 0.6117 0.0388 Uiso 1 8 calc
H7B H 0.8389 0.8454 0.4785 0.0388 Uiso 1 8 calc
H7C H 0.9031 0.766 0.5706 0.0388 Uiso 1 8 calc
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Mo Mo -1.6832 0.6857
;
International Tables for Crystallography
(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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Mo1 N3 180.000 yes . .
N1 Mo1 C1 87.26(12) yes . .
N1 Mo1 C1 87.26(12) yes . 2_655
N1 Mo1 C1 87.26(12) yes . 3_665
N1 Mo1 C1 87.26(12) yes . 4_565
N3 Mo1 C1 92.74(12) yes . .
N3 Mo1 C1 92.74(12) yes . 2_655
N3 Mo1 C1 92.74(12) yes . 3_665
N3 Mo1 C1 92.74(12) yes . 4_565
C1 Mo1 C1 89.87(12) yes . 2_655
C1 Mo1 C1 174.52(17) yes . 3_665
C1 Mo1 C1 89.87(12) yes . 4_565
C1 Mo1 C1 89.87(12) yes 2_655 3_665
C1 Mo1 C1 174.52(17) yes 2_655 4_565
C1 Mo1 C1 89.87(12) yes 3_665 4_565
Mo1 N1 N2 180.000 yes . .
Mo1 N3 N4 180.000(6) yes . .
C1 N5 C2 112.7(3) yes . .
C1 N5 C4 125.6(3) yes . .
C2 N5 C4 121.5(3) yes . .
C1 N6 C3 112.5(3) yes . .
C1 N6 C5 124.2(3) yes . .
C3 N6 C5 123.2(3) yes . .
Mo1 C1 N5 129.1(3) yes . .
Mo1 C1 N6 128.7(2) yes . .
N5 C1 N6 101.5(3) yes . .
N5 C2 C3 106.7(3) yes . .
N5 C2 C6 122.6(3) yes . .
C3 C2 C6 130.6(3) yes . .
N6 C3 C2 106.6(3) yes . .
N6 C3 C7 121.9(3) yes . .
C2 C3 C7 131.5(3) yes . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Mo1 N1 1.977(9) yes .
Mo1 N3 1.999(11) yes .
Mo1 C1 2.216(3) yes .
Mo1 C1 2.216(3) yes 2_655
Mo1 C1 2.216(3) yes 3_665
Mo1 C1 2.216(3) yes 4_565
N1 N2 1.135(13) yes .
N3 N4 1.139(15) yes .
N5 C1 1.379(4) yes .
N5 C2 1.402(5) yes .
N5 C4 1.446(5) yes .
N6 C1 1.385(4) yes .
N6 C3 1.404(4) yes .
N6 C5 1.450(5) yes .
C2 C3 1.337(6) yes .
C2 C6 1.491(6) yes .
C3 C7 1.490(5) yes .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_2
Mo1 N5 3.265(3) no 2_655
Mo1 N5 3.265(3) no 3_665
Mo1 N5 3.265(3) no 4_565
Mo1 N6 3.266(3) no 2_655
Mo1 N6 3.266(3) no 3_665
Mo1 N6 3.266(3) no 4_565
N1 N5 3.263(4) no .
N1 N5 3.263(4) no 2_655
N1 N5 3.263(4) no 3_665
N1 N5 3.263(4) no 4_565
N1 C4 3.174(4) no .
N1 C4 3.174(4) no 2_655
N1 C4 3.174(4) no 3_665
N1 C4 3.174(4) no 4_565
N2 C4 3.409(5) no .
N2 C4 3.409(5) no 2_655
N2 C4 3.409(5) no 3_665
N2 C4 3.409(5) no 4_565
N3 N6 3.528(5) no .
N3 N6 3.528(5) no 2_655
N3 N6 3.528(5) no 3_665
N3 N6 3.528(5) no 4_565
N3 C5 3.286(4) no .
N3 C5 3.286(4) no 2_655
N3 C5 3.286(4) no 3_665
N3 C5 3.286(4) no 4_565
N5 C1 3.529(5) no 2_655
N5 C5 3.554(5) no .
N5 C5 3.562(6) no 2_655
N6 C1 3.473(5) no 4_565
N6 C4 3.555(4) no .
N6 C4 3.326(4) no 4_565
C1 C4 3.213(5) no 4_565
C1 C5 3.261(6) no 2_655
C2 C5 3.588(6) no .
C3 C4 3.574(5) no .
C4 C6 2.966(5) no .
C5 C7 2.986(5) no .
C6 C7 3.294(6) no .
N2 C7 3.373(7) no 5_645
N2 C7 3.373(7) no 6_445
N2 C7 3.373(7) no 7_465
N2 C7 3.373(7) no 8_665
C5 C6 3.365(6) no 5_644
C6 C5 3.365(6) no 5_655
C7 N2 3.373(7) no 5_654
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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N1 Mo1 C1 N5 -37.9(3) no . . .
N1 Mo1 C1 N6 130.6(3) no . . .
N1 Mo1 C1 N5 -37.9(3) no . 2_655 2_655
N1 Mo1 C1 N6 130.6(3) no . 2_655 2_655
N1 Mo1 C1 N5 -37.9(3) no . 3_665 3_665
N1 Mo1 C1 N6 130.6(3) no . 3_665 3_665
N1 Mo1 C1 N5 -37.9(3) no . 4_565 4_565
N1 Mo1 C1 N6 130.6(3) no . 4_565 4_565
N3 Mo1 C1 N5 142.1(3) no . . .
N3 Mo1 C1 N6 -49.4(3) no . . .
N3 Mo1 C1 N5 142.1(3) no . 2_655 2_655
N3 Mo1 C1 N6 -49.4(3) no . 2_655 2_655
N3 Mo1 C1 N5 142.1(3) no . 3_665 3_665
N3 Mo1 C1 N6 -49.4(3) no . 3_665 3_665
N3 Mo1 C1 N5 142.1(3) no . 4_565 4_565
N3 Mo1 C1 N6 -49.4(3) no . 4_565 4_565
C1 Mo1 C1 N5 -125.2(3) no . 2_655 2_655
C1 Mo1 C1 N6 43.4(3) no . 2_655 2_655
C1 Mo1 C1 N5 49.4(3) no 2_655 . .
C1 Mo1 C1 N6 -142.1(3) no 2_655 . .
C1 Mo1 C1 N5 49.4(3) no . 4_565 4_565
C1 Mo1 C1 N6 -142.1(3) no . 4_565 4_565
C1 Mo1 C1 N5 -125.2(3) no 4_565 . .
C1 Mo1 C1 N6 43.4(3) no 4_565 . .
C1 Mo1 C1 N5 -125.2(3) no 2_655 3_665 3_665
C1 Mo1 C1 N6 43.4(3) no 2_655 3_665 3_665
C1 Mo1 C1 N5 49.4(3) no 3_665 2_655 2_655
C1 Mo1 C1 N6 -142.1(3) no 3_665 2_655 2_655
C1 Mo1 C1 N5 -125.2(3) no 3_665 4_565 4_565
C1 Mo1 C1 N6 43.4(3) no 3_665 4_565 4_565
C1 Mo1 C1 N5 49.4(3) no 4_565 3_665 3_665
C1 Mo1 C1 N6 -142.1(3) no 4_565 3_665 3_665
C1 N5 C2 C3 0.2(4) no . . .
C1 N5 C2 C6 -177.6(3) no . . .
C2 N5 C1 Mo1 169.5(3) no . . .
C2 N5 C1 N6 -1.4(4) no . . .
C4 N5 C1 Mo1 -15.4(5) no . . .
C4 N5 C1 N6 173.7(3) no . . .
C4 N5 C2 C3 -175.1(3) no . . .
C4 N5 C2 C6 7.0(5) no . . .
C1 N6 C3 C2 -2.1(4) no . . .
C1 N6 C3 C7 176.5(3) no . . .
C3 N6 C1 Mo1 -168.8(3) no . . .
C3 N6 C1 N5 2.1(4) no . . .
C5 N6 C1 Mo1 7.8(5) no . . .
C5 N6 C1 N5 178.7(3) no . . .
C5 N6 C3 C2 -178.8(3) no . . .
C5 N6 C3 C7 -0.2(5) no . . .
N5 C2 C3 N6 1.1(4) no . . .
N5 C2 C3 C7 -177.3(4) no . . .
C6 C2 C3 N6 178.7(4) no . . .
C6 C2 C3 C7 0.3(8) no . . .
