#------------------------------------------------------------------------------
#$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $
#$Revision: 264242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/65/4326571.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_4326571
loop_
_publ_author_name
'Treffly B. Ditri'
'Curtis E. Moore'
'Arnold L. Rheingold'
'Joshua S. Figueroa'
_publ_section_title
;
 Oxidative Decarbonylation of m-Terphenyl Isocyanide Complexes of
 Molybdenum and Tungsten: Precursors to Low-Coordinate Isocyanide
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10448
_journal_page_last               10459
_journal_paper_doi               10.1021/ic2015868
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C78 H94 I4 Mo N2'
_chemical_formula_weight         1663.10
_chemical_name_common            trans-MoI4(CNArDipp2)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/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                 126.228(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.601(5)
_cell_length_b                   16.167(4)
_cell_length_c                   15.491(7)
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.45
_cell_volume                     4162(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19075
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_platon_squeeze_details
; 
SQUEEZE was employed to account for severely disordered molecules of Tol 
(C7H8).  A total of 221 electrons in a solvent accessible void of 
724.0 Ang^3 were accounted for.  This corresponds to roughly 4 
disordered molecules of Tol per unit cell. 
;
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0579P)²+4.8892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                3822
_reflns_number_total             4747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015868_si_001_06.cif
_cod_data_source_block           jfig217
_cod_depositor_comments
;

2021-04-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         831.55
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C39 H47 I2 Mo0.50 N'
_cod_database_code               4326571
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.0000 0.5000 0.0000 0.02305(16) Uani 1 4 d S
I2 I 0.0000 0.33065(2) 0.0000 0.04020(14) Uani 1 2 d S
I1 I 0.14261(3) 0.5000 0.03544(3) 0.04798(15) Uani 1 2 d S
N1 N 0.0857(2) 0.5000 0.2596(3) 0.0183(8) Uani 1 2 d S
C2 C 0.1241(3) 0.5000 0.3705(3) 0.0160(9) Uani 1 2 d S
C15 C 0.2572(3) 0.5000 0.3937(4) 0.0201(10) Uani 1 2 d S
C8 C -0.0145(3) 0.5000 0.3305(4) 0.0195(10) Uani 1 2 d S
C20 C 0.2570(2) 0.3413(2) 0.3961(3) 0.0261(8) Uani 1 1 d .
H20 H 0.2158 0.3522 0.4093 0.031 Uiso 1 1 calc R
C13 C -0.0127(2) 0.6590(2) 0.3351(3) 0.0242(7) Uani 1 1 d .
H13 H 0.0404 0.6491 0.4054 0.029 Uiso 1 1 calc R
C16 C 0.2799(2) 0.4241(2) 0.3742(3) 0.0229(7) Uani 1 1 d .
C9 C -0.0564(2) 0.5759(2) 0.2944(3) 0.0216(7) Uani 1 1 d .
C1 C 0.0564(3) 0.5000 0.1691(4) 0.0212(10) Uani 1 2 d S
C10 C -0.1400(2) 0.5741(2) 0.2186(3) 0.0267(8) Uani 1 1 d .
H10 H -0.1692 0.6246 0.1933 0.032 Uiso 1 1 calc R
C7 C 0.0763(3) 0.5000 0.4080(4) 0.0183(9) Uani 1 2 d S
C6 C 0.1164(3) 0.5000 0.5186(4) 0.0233(10) Uani 1 2 d S
H6 H 0.0862 0.5000 0.5470 0.028 Uiso 1 2 calc SR
C17 C 0.3277(2) 0.4259(2) 0.3375(3) 0.0300(8) Uani 1 1 d .
H17 H 0.3441 0.3751 0.3248 0.036 Uiso 1 1 calc R
C4 C 0.2455(3) 0.5000 0.5475(4) 0.0251(11) Uani 1 2 d S
H4 H 0.3026 0.5000 0.5957 0.030 Uiso 1 2 calc SR
C3 C 0.2085(3) 0.5000 0.4379(4) 0.0172(9) Uani 1 2 d S
C21 C 0.2198(3) 0.2810(3) 0.3015(3) 0.0374(9) Uani 1 1 d .
H21A H 0.1720 0.3063 0.2379 0.056 Uiso 1 1 calc R
H21B H 0.2044 0.2298 0.3190 0.056 Uiso 1 1 calc R
H21C H 0.2592 0.2685 0.2872 0.056 Uiso 1 1 calc R
C19 C 0.3308(2) 0.3032(3) 0.4984(3) 0.0340(9) Uani 1 1 d .
H19A H 0.3746 0.2976 0.4908 0.051 Uiso 1 1 calc R
H19B H 0.3168 0.2486 0.5102 0.051 Uiso 1 1 calc R
H19C H 0.3482 0.3392 0.5594 0.051 Uiso 1 1 calc R
C18 C 0.3519(3) 0.5000 0.3191(5) 0.0329(12) Uani 1 2 d S
H18 H 0.3844 0.5000 0.2943 0.039 Uiso 1 2 calc SR
C14 C -0.0594(3) 0.7216(2) 0.3533(3) 0.0341(9) Uani 1 1 d .
H14A H -0.1093 0.7367 0.2843 0.051 Uiso 1 1 calc R
H14B H -0.0264 0.7712 0.3878 0.051 Uiso 1 1 calc R
H14C H -0.0722 0.6970 0.3993 0.051 Uiso 1 1 calc R
C11 C -0.1805(3) 0.5000 0.1801(4) 0.0289(11) Uani 1 2 d S
H11 H -0.2370 0.5000 0.1264 0.035 Uiso 1 2 calc SR
C5 C 0.2003(3) 0.5000 0.5881(4) 0.0279(11) Uani 1 2 d S
H5 H 0.2268 0.5000 0.6633 0.033 Uiso 1 2 calc SR
C12 C 0.0035(3) 0.6948(2) 0.2585(3) 0.0341(9) Uani 1 1 d .
H12A H 0.0395 0.6578 0.2548 0.051 Uiso 1 1 calc R
H12B H 0.0289 0.7493 0.2843 0.051 Uiso 1 1 calc R
H12C H -0.0474 0.7005 0.1871 0.051 Uiso 1 1 calc R
C24 C 0.0536(3) 0.0846(3) 0.2000(4) 0.0469(11) Uani 1 1 d .
H24 H 0.0530 0.1433 0.1996 0.056 Uiso 1 1 calc R
C23 C 0.0835(3) 0.0434(3) 0.1530(3) 0.0405(10) Uani 1 1 d .
C25 C 0.0248(3) 0.0426(3) 0.2475(4) 0.0546(13) Uani 1 1 d .
H25 H 0.0049 0.0721 0.2804 0.066 Uiso 1 1 calc R
C22 C 0.1125(7) 0.0856(6) 0.1043(8) 0.135(4) Uani 1 1 d .
H22A H 0.1116 0.1452 0.1151 0.202 Uiso 1 1 calc R
H22B H 0.0785 0.0734 0.0275 0.202 Uiso 1 1 calc R
H22C H 0.1678 0.0681 0.1360 0.202 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
C1 Mo1 C1 180.0 . 5_565
C1 Mo1 I1 89.26(13) . 5_565
C1 Mo1 I1 90.74(13) 5_565 5_565
C1 Mo1 I1 90.74(13) . .
C1 Mo1 I1 89.26(13) 5_565 .
I1 Mo1 I1 180.0 5_565 .
C1 Mo1 I2 90.0 . 5_565
C1 Mo1 I2 90.0 5_565 5_565
I1 Mo1 I2 90.0 5_565 5_565
I1 Mo1 I2 90.0 . 5_565
C1 Mo1 I2 90.0 . .
C1 Mo1 I2 90.0 5_565 .
I1 Mo1 I2 90.0 5_565 .
I1 Mo1 I2 90.0 . .
I2 Mo1 I2 180.0 5_565 .
C1 N1 C2 177.9(5) . .
N1 C2 C3 117.8(4) . .
N1 C2 C7 118.6(4) . .
C3 C2 C7 123.6(4) . .
C16 C15 C16 121.2(4) . 6_565
C16 C15 C3 119.4(2) . .
C16 C15 C3 119.4(2) 6_565 .
C9 C8 C9 120.8(4) . 6_565
C9 C8 C7 119.6(2) . .
C9 C8 C7 119.6(2) 6_565 .
C16 C20 C19 109.5(3) . .
C16 C20 C21 113.1(3) . .
C19 C20 C21 111.2(3) . .
C16 C20 H20 107.6 . .
C19 C20 H20 107.6 . .
C21 C20 H20 107.6 . .
C12 C13 C9 111.0(3) . .
C12 C13 C14 109.9(3) . .
C9 C13 C14 112.1(3) . .
C12 C13 H13 107.9 . .
C9 C13 H13 107.9 . .
C14 C13 H13 107.9 . .
C17 C16 C15 118.2(3) . .
C17 C16 C20 119.5(3) . .
C15 C16 C20 122.2(3) . .
C10 C9 C8 118.4(3) . .
C10 C9 C13 119.8(3) . .
C8 C9 C13 121.8(3) . .
N1 C1 Mo1 179.1(4) . .
C11 C10 C9 120.8(4) . .
C11 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
C6 C7 C2 117.1(4) . .
C6 C7 C8 122.2(4) . .
C2 C7 C8 120.7(4) . .
C7 C6 C5 120.9(4) . .
C7 C6 H6 119.6 . .
C5 C6 H6 119.6 . .
C18 C17 C16 121.6(3) . .
C18 C17 H17 119.2 . .
C16 C17 H17 119.2 . .
C3 C4 C5 121.3(5) . .
C3 C4 H4 119.4 . .
C5 C4 H4 119.4 . .
C4 C3 C2 116.9(4) . .
C4 C3 C15 121.5(4) . .
C2 C3 C15 121.6(4) . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C20 C19 H19A 109.5 . .
C20 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C20 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C17 C18 C17 119.1(5) 6_565 .
C17 C18 H18 120.4 6_565 .
C17 C18 H18 120.4 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C10 C11 C10 120.8(5) . 6_565
C10 C11 H11 119.6 . .
C10 C11 H11 119.6 6_565 .
C6 C5 C4 120.2(4) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C13 C12 H12A 109.5 . .
C13 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C13 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C25 C24 C23 121.3(5) . .
C25 C24 H24 119.4 . .
C23 C24 H24 119.4 . .
C24 C23 C22 121.5(5) . .
C24 C23 C23 119.0(3) . 6
C22 C23 C23 119.5(4) . 6
C24 C25 C25 119.7(3) . 6
C24 C25 H25 120.1 . .
C25 C25 H25 120.1 6 .
C23 C22 H22A 109.5 . .
C23 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C23 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C1 2.148(5) .
Mo1 C1 2.148(5) 5_565
Mo1 I1 2.6507(8) 5_565
Mo1 I1 2.6508(8) .
Mo1 I2 2.7379(8) 5_565
Mo1 I2 2.7379(7) .
N1 C1 1.153(6) .
N1 C2 1.403(5) .
C2 C3 1.403(7) .
C2 C7 1.409(6) .
C15 C16 1.408(4) .
C15 C16 1.408(4) 6_565
C15 C3 1.511(6) .
C8 C9 1.411(4) .
C8 C9 1.411(4) 6_565
C8 C7 1.512(7) .
C20 C16 1.522(5) .
C20 C19 1.534(5) .
C20 C21 1.535(5) .
C20 H20 1.0000 .
C13 C12 1.525(5) .
C13 C9 1.529(5) .
C13 C14 1.534(5) .
C13 H13 1.0000 .
C16 C17 1.399(5) .
C9 C10 1.399(5) .
C10 C11 1.378(5) .
C10 H10 0.9500 .
C7 C6 1.394(6) .
C6 C5 1.396(7) .
C6 H6 0.9500 .
C17 C18 1.390(5) .
C17 H17 0.9500 .
C4 C3 1.390(6) .
C4 C5 1.398(7) .
C4 H4 0.9500 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C18 C17 1.390(5) 6_565
C18 H18 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C11 C10 1.378(5) 6_565
C11 H11 0.9500 .
C5 H5 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C24 C25 1.367(7) .
C24 C23 1.372(7) .
C24 H24 0.9500 .
C23 C22 1.386(11) .
C23 C23 1.404(9) 6
C25 C25 1.379(11) 6
C25 H25 0.9500 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.026 -0.026 0.000 269 81 ' '
2 0.024 0.284 0.338 25 4 ' '
3 0.026 0.026 0.500 269 81 ' '
4 -0.024 0.716 0.838 25 4 ' '
5 0.216 0.524 0.088 25 4 ' '
6 0.284 1.024 0.662 25 4 ' '
7 0.474 0.526 0.250 269 81 ' '
8 0.526 0.474 0.750 269 81 ' '
9 0.476 0.784 0.412 25 4 ' '
10 0.524 0.216 0.912 25 4 ' '
11 0.716 0.976 0.162 25 4 ' '
12 0.784 0.476 0.588 25 4 ' '
