#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/05/7010502.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_7010502
loop_
_publ_author_name
'Adams, Christopher J.'
'Anderson, Kirsty M.'
'Bartlett, Ian M.'
'Connelly, Neil G.'
'Orpen, A. Guy'
'Paget, Timothy J.'
'Phetmung, Hirihattaya'
'Smith, David W.'
_publ_section_title
;
 Molybdenum-based alkyne--isocyanide coupling reactions: synthesis of a
 reactive diiminometallacyclopentene complex
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1284
_journal_paper_doi               10.1039/b010018h
_journal_year                    2001
_chemical_formula_sum            'C32 H28 N2'
_chemical_formula_weight         440.56
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.475(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8714(11)
_cell_length_b                   14.597(2)
_cell_length_c                   19.138(3)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    173(2)
_cell_volume                     2477.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD area detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13017
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.767853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.127
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+0.1085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3415
_reflns_number_total             4376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b010018h.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2477.6(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010502
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.07910(12) 0.72635(7) 0.10803(5) 0.0332(3) Uani 1 1 d . . .
N2 N 0.17289(12) 0.66980(7) 0.26826(5) 0.0315(3) Uani 1 1 d . . .
C2 C 0.02341(13) 0.76794(9) 0.04516(6) 0.0313(3) Uani 1 1 d . . .
C3 C 0.07736(14) 0.85380(9) 0.02549(6) 0.0343(3) Uani 1 1 d . . .
C4 C 0.18869(16) 0.90497(10) 0.07147(7) 0.0448(3) Uani 1 1 d . . .
H4A H 0.2730 0.8645 0.0844 0.067 Uiso 1 1 calc R . .
H4B H 0.1390 0.9255 0.1138 0.067 Uiso 1 1 calc R . .
H4C H 0.2266 0.9582 0.0462 0.067 Uiso 1 1 calc R . .
C5 C 0.02709(16) 0.88908(10) -0.03842(7) 0.0418(3) Uani 1 1 d . . .
H5A H 0.0614 0.9476 -0.0528 0.050 Uiso 1 1 calc R . .
C6 C -0.07200(17) 0.84054(11) -0.08153(7) 0.0460(4) Uani 1 1 d . . .
H6A H -0.1068 0.8662 -0.1246 0.055 Uiso 1 1 calc R . .
C7 C -0.11981(16) 0.75505(10) -0.06161(7) 0.0430(4) Uani 1 1 d . . .
H7A H -0.1860 0.7216 -0.0919 0.052 Uiso 1 1 calc R . .
C8 C -0.07357(14) 0.71643(9) 0.00177(7) 0.0361(3) Uani 1 1 d . . .
C9 C -0.12345(18) 0.62235(10) 0.02383(8) 0.0494(4) Uani 1 1 d . . .
H9A H -0.0350 0.5857 0.0375 0.074 Uiso 1 1 calc R . .
H9B H -0.1775 0.5925 -0.0152 0.074 Uiso 1 1 calc R . .
H9C H -0.1903 0.6277 0.0636 0.074 Uiso 1 1 calc R . .
C10 C 0.27270(14) 0.62468(8) 0.22119(6) 0.0309(3) Uani 1 1 d . . .
C11 C 0.40882(15) 0.66690(9) 0.20551(7) 0.0366(3) Uani 1 1 d . . .
C12 C 0.44752(18) 0.75965(11) 0.23434(8) 0.0516(4) Uani 1 1 d . . .
H12A H 0.4430 0.7582 0.2854 0.077 Uiso 1 1 calc R . .
H12B H 0.3753 0.8049 0.2158 0.077 Uiso 1 1 calc R . .
H12C H 0.5495 0.7765 0.2207 0.077 Uiso 1 1 calc R . .
C13 C 0.50431(16) 0.62177(11) 0.16011(7) 0.0488(4) Uani 1 1 d . . .
H13A H 0.5970 0.6496 0.1483 0.059 Uiso 1 1 calc R . .
C14 C 0.46705(19) 0.53779(12) 0.13212(8) 0.0539(4) Uani 1 1 d . . .
H14A H 0.5333 0.5082 0.1011 0.065 Uiso 1 1 calc R . .
C15 C 0.33312(19) 0.49676(10) 0.14930(8) 0.0504(4) Uani 1 1 d . . .
H15A H 0.3087 0.4383 0.1303 0.060 Uiso 1 1 calc R . .
C16 C 0.23291(16) 0.53898(9) 0.19379(7) 0.0389(3) Uani 1 1 d . . .
C17 C 0.08333(19) 0.49690(11) 0.20958(9) 0.0586(4) Uani 1 1 d . . .
H17A H 0.0734 0.4918 0.2603 0.088 Uiso 1 1 calc R . .
H17B H 0.0767 0.4358 0.1885 0.088 Uiso 1 1 calc R . .
H17C H 0.0022 0.5356 0.1903 0.088 Uiso 1 1 calc R . .
C18 C 0.07397(13) 0.72126(8) 0.23990(6) 0.0288(3) Uani 1 1 d . . .
C19 C -0.04443(13) 0.78450(8) 0.26546(6) 0.0287(3) Uani 1 1 d . . .
C20 C -0.07975(13) 0.81563(8) 0.19881(6) 0.0294(3) Uani 1 1 d . . .
C21 C 0.03110(14) 0.75155(8) 0.16671(6) 0.0293(3) Uani 1 1 d . . .
C22 C -0.17923(13) 0.88691(8) 0.16938(6) 0.0310(3) Uani 1 1 d . . .
C23 C -0.17908(16) 0.97456(9) 0.19877(7) 0.0397(3) Uani 1 1 d . . .
H23A H -0.1145 0.9879 0.2378 0.048 Uiso 1 1 calc R . .
C24 C -0.27280(18) 1.04190(10) 0.17111(8) 0.0517(4) Uani 1 1 d . . .
H24A H -0.2714 1.1016 0.1909 0.062 Uiso 1 1 calc R . .
C25 C -0.36839(18) 1.02283(11) 0.11479(8) 0.0534(4) Uani 1 1 d . . .
H25A H -0.4344 1.0688 0.0968 0.064 Uiso 1 1 calc R . .
C26 C -0.36781(16) 0.93692(11) 0.08483(8) 0.0460(4) Uani 1 1 d . . .
H26A H -0.4329 0.9239 0.0459 0.055 Uiso 1 1 calc R . .
C27 C -0.27265(14) 0.86958(9) 0.11132(7) 0.0359(3) Uani 1 1 d . . .
H27A H -0.2710 0.8110 0.0897 0.043 Uiso 1 1 calc R . .
C28 C -0.09697(13) 0.80207(8) 0.33585(6) 0.0293(3) Uani 1 1 d . . .
C29 C -0.01497(15) 0.76618(9) 0.39269(7) 0.0358(3) Uani 1 1 d . . .
H29A H 0.0710 0.7290 0.3851 0.043 Uiso 1 1 calc R . .
C30 C -0.05875(17) 0.78464(10) 0.46033(7) 0.0437(4) Uani 1 1 d . . .
H30A H -0.0010 0.7613 0.4988 0.052 Uiso 1 1 calc R . .
C31 C -0.18549(16) 0.83668(10) 0.47216(7) 0.0433(4) Uani 1 1 d . . .
H31A H -0.2146 0.8494 0.5186 0.052 Uiso 1 1 calc R . .
C32 C -0.26990(15) 0.87017(9) 0.41590(7) 0.0391(3) Uani 1 1 d . . .
H32A H -0.3586 0.9047 0.4239 0.047 Uiso 1 1 calc R . .
C33 C -0.22613(14) 0.85382(9) 0.34837(7) 0.0345(3) Uani 1 1 d . . .
H33A H -0.2841 0.8779 0.3102 0.041 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'
N N 0.0061 0.0033 '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
C21 N1 C2 120.54(11) . . ?
C18 N2 C10 115.71(10) . . ?
C3 C2 C8 122.14(12) . . ?
C3 C2 N1 119.75(11) . . ?
C8 C2 N1 117.82(12) . . ?
C5 C3 C2 117.72(12) . . ?
C5 C3 C4 121.45(12) . . ?
C2 C3 C4 120.82(11) . . ?
C6 C5 C3 121.26(14) . . ?
C7 C6 C5 119.65(13) . . ?
C6 C7 C8 121.60(13) . . ?
C7 C8 C2 117.57(13) . . ?
C7 C8 C9 122.15(13) . . ?
C2 C8 C9 120.27(12) . . ?
C11 C10 C16 121.74(12) . . ?
C11 C10 N2 118.84(11) . . ?
C16 C10 N2 119.40(11) . . ?
C13 C11 C10 117.93(13) . . ?
C13 C11 C12 121.28(13) . . ?
C10 C11 C12 120.75(12) . . ?
C14 C13 C11 121.35(15) . . ?
C13 C14 C15 119.66(14) . . ?
C14 C15 C16 121.48(14) . . ?
C15 C16 C10 117.84(14) . . ?
C15 C16 C17 121.64(13) . . ?
C10 C16 C17 120.45(13) . . ?
N2 C18 C19 135.47(11) . . ?
N2 C18 C21 136.66(11) . . ?
C19 C18 C21 87.72(9) . . ?
C20 C19 C28 136.36(12) . . ?
C20 C19 C18 92.61(10) . . ?
C28 C19 C18 131.02(11) . . ?
C19 C20 C22 134.99(11) . . ?
C19 C20 C21 92.14(10) . . ?
C22 C20 C21 132.78(11) . . ?
N1 C21 C20 141.58(12) . . ?
N1 C21 C18 131.01(11) . . ?
C20 C21 C18 87.42(9) . . ?
C27 C22 C23 118.80(12) . . ?
C27 C22 C20 121.16(12) . . ?
C23 C22 C20 120.03(12) . . ?
C24 C23 C22 120.14(14) . . ?
C25 C24 C23 120.37(14) . . ?
C26 C25 C24 119.90(14) . . ?
C25 C26 C27 120.17(14) . . ?
C26 C27 C22 120.57(13) . . ?
C29 C28 C33 118.84(11) . . ?
C29 C28 C19 118.76(11) . . ?
C33 C28 C19 122.39(11) . . ?
C30 C29 C28 120.11(13) . . ?
C31 C30 C29 120.57(13) . . ?
C30 C31 C32 119.56(12) . . ?
C33 C32 C31 120.50(13) . . ?
C32 C33 C28 120.37(13) . . ?
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
N1 C21 1.2659(16) . ?
N1 C2 1.4248(15) . ?
N2 C18 1.2666(16) . ?
N2 C10 1.4389(15) . ?
C2 C3 1.3967(18) . ?
C2 C8 1.3994(18) . ?
C3 C5 1.3900(18) . ?
C3 C4 1.5043(19) . ?
C5 C6 1.385(2) . ?
C6 C7 1.375(2) . ?
C7 C8 1.3899(19) . ?
C8 C9 1.506(2) . ?
C10 C11 1.3952(18) . ?
C10 C16 1.3982(18) . ?
C11 C13 1.3944(19) . ?
C11 C12 1.498(2) . ?
C13 C14 1.375(2) . ?
C14 C15 1.378(2) . ?
C15 C16 1.391(2) . ?
C16 C17 1.500(2) . ?
C18 C19 1.4905(17) . ?
C18 C21 1.5081(17) . ?
C19 C20 1.3826(17) . ?
C19 C28 1.4594(17) . ?
C20 C22 1.4672(17) . ?
C20 C21 1.5002(17) . ?
C22 C27 1.3922(18) . ?
C22 C23 1.3977(18) . ?
C23 C24 1.384(2) . ?
C24 C25 1.383(2) . ?
C25 C26 1.379(2) . ?
C26 C27 1.3834(19) . ?
C28 C29 1.3951(18) . ?
C28 C33 1.3982(18) . ?
C29 C30 1.3875(18) . ?
C30 C31 1.380(2) . ?
C31 C32 1.385(2) . ?
C32 C33 1.3798(18) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652732
