#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/30/4303091.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_4303091
loop_
_publ_author_name
'Treffly B. Ditri'
'Brian J. Fox'
'Curtis E. Moore'
'Arnold L. Rheingold'
'Joshua S. Figueroa'
_publ_section_title
;
Effective Control of Ligation and Geometric Isomerism: Direct Comparison of
Steric Properties Associated with Bis-mesityl and
Bis-diisopropylphenyl m-Terphenyl Isocyanides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8362
_journal_page_last               8375
_journal_paper_doi               10.1021/ic9010828
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C65.5 H74 Mo N2.25 O3'
_chemical_formula_weight         1036.71
_chemical_name_common            Mo(NCMe)(CO)3(CNArDipp2)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7048(5)
_cell_length_b                   20.7048(5)
_cell_length_c                   19.9285(6)
_cell_measurement_reflns_used    6751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.30
_cell_measurement_theta_min      3.02
_cell_volume                     8543.1(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.971
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19787
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         65.97
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.7548
_exptl_absorpt_correction_T_min  0.7255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2195
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00004(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0699
_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)+(0.1617P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2389
_reflns_number_gt                2555
_reflns_number_total             3739
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic9010828_si_002_09.cif
_cod_data_source_block           jfig180
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_formula_sum        'C65.50 H74 Mo N2.25 O3'
_cod_database_code               4303091
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-y, x, -z'
'x, y, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'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
C1 C 0.5246(2) 0.9025(2) 0.0000 0.0606(12) Uani 1 2 d S . .
C2 C 0.5538(2) 0.78425(18) 0.0000 0.0478(9) Uani 1 2 d S . .
C3 C 0.61854(19) 0.76455(19) 0.0000 0.0479(9) Uani 1 2 d S . .
C4 C 0.6305(2) 0.6997(2) 0.0000 0.0597(11) Uani 1 2 d S . .
H4 H 0.6740 0.6851 0.0000 0.072 Uiso 1 2 calc SR . .
C5 C 0.5816(2) 0.6551(2) 0.0000 0.0798(17) Uani 1 2 d S . .
H5 H 0.5913 0.6103 0.0000 0.096 Uiso 1 2 calc SR . .
C6 C 0.5173(2) 0.6762(2) 0.0000 0.0743(15) Uani 1 2 d S . .
H6 H 0.4834 0.6452 0.0000 0.089 Uiso 1 2 calc SR . .
C7 C 0.50245(19) 0.74031(19) 0.0000 0.0510(10) Uani 1 2 d S . .
C8 C 0.4345(2) 0.7641(2) 0.0000 0.0568(11) Uani 1 2 d S . .
C9 C 0.40291(16) 0.77610(16) -0.0606(2) 0.0644(9) Uani 1 1 d . . .
C10 C 0.34006(18) 0.79909(17) -0.0590(2) 0.0731(10) Uani 1 1 d . . .
H10 H 0.3182 0.8069 -0.1001 0.088 Uiso 1 1 calc R . .
C11 C 0.3087(3) 0.8108(2) 0.0000 0.0784(16) Uani 1 2 d S . .
H11 H 0.2657 0.8268 0.0000 0.094 Uiso 1 2 calc SR . .
C12 C 0.4351(2) 0.7649(2) -0.1269(2) 0.0837(12) Uani 1 1 d . . .
H12 H 0.4801 0.7502 -0.1171 0.100 Uiso 1 1 calc R . .
C13 C 0.4408(3) 0.8269(3) -0.1676(3) 0.126(2) Uani 1 1 d . . .
H13A H 0.3981 0.8391 -0.1847 0.189 Uiso 1 1 calc R . .
H13B H 0.4703 0.8200 -0.2054 0.189 Uiso 1 1 calc R . .
H13C H 0.4575 0.8615 -0.1390 0.189 Uiso 1 1 calc R . .
C14 C 0.4030(3) 0.7116(3) -0.1659(3) 0.126(2) Uani 1 1 d . . .
H14A H 0.4205 0.6699 -0.1516 0.188 Uiso 1 1 calc R . .
H14B H 0.4112 0.7178 -0.2139 0.188 Uiso 1 1 calc R . .
H14C H 0.3564 0.7126 -0.1576 0.188 Uiso 1 1 calc R . .
C15 C 0.6721(2) 0.8127(2) 0.0000 0.0525(10) Uani 1 2 d S . .
C16 C 0.6970(2) 0.83530(18) 0.0610(2) 0.0773(11) Uani 1 1 d . . .
C17 C 0.7469(2) 0.8798(3) 0.0595(3) 0.1110(18) Uani 1 1 d . . .
H17 H 0.7638 0.8961 0.1005 0.133 Uiso 1 1 calc R . .
C18 C 0.7720(4) 0.9006(4) 0.0000 0.118(3) Uani 1 2 d S . .
H18 H 0.8074 0.9299 0.0000 0.142 Uiso 1 2 calc SR . .
C19 C 0.6688(3) 0.8153(2) 0.1275(2) 0.1082(18) Uani 1 1 d . . .
H19 H 0.6411 0.7765 0.1198 0.130 Uiso 1 1 calc R . .
C20 C 0.6259(3) 0.8690(4) 0.1581(3) 0.137(2) Uani 1 1 d . . .
H20A H 0.6096 0.8548 0.2018 0.205 Uiso 1 1 calc R . .
H20B H 0.5895 0.8777 0.1280 0.205 Uiso 1 1 calc R . .
H20C H 0.6516 0.9084 0.1638 0.205 Uiso 1 1 calc R . .
C21 C 0.7204(4) 0.7973(3) 0.1774(3) 0.141(3) Uani 1 1 d . . .
H21A H 0.7393 0.8366 0.1964 0.212 Uiso 1 1 calc R . .
H21B H 0.7541 0.7722 0.1548 0.212 Uiso 1 1 calc R . .
H21C H 0.7013 0.7713 0.2134 0.212 Uiso 1 1 calc R . .
C1OA C 0.5000 1.0000 0.1042(7) 0.088(3) Uani 0.13 2 d SPDU A 1
C2OA C 0.5859(7) 1.0218(7) 0.0445(9) 0.076(3) Uani 0.25 1 d PDU . 1
C1OB C 0.5428(9) 1.0075(6) 0.0903(7) 0.061(3) Uani 0.22 1 d PDU . 2
C2OB C 0.5961(5) 1.0211(5) 0.0000 0.064(3) Uani 0.44 2 d SPDU A 2
C1S C 0.5000 1.0000 0.1656(7) 0.106(4) Uani 0.13 2 d SPDU A 3
C2S C 0.5000 1.0000 0.2500 0.114(6) Uani 0.25 4 d SPDU A 3
Mo1 Mo 0.5000 1.0000 0.0000 0.0820(4) Uani 1 4 d SD . .
N1 N 0.53982(17) 0.84969(17) 0.0000 0.0509(8) Uani 1 2 d S . .
N1S N 0.5000 1.0000 0.1042(7) 0.088(3) Uani 0.13 2 d SPU A 3
O1A O 0.5000 1.0000 0.1656(7) 0.106(4) Uani 0.13 2 d SPDU A 1
O2A O 0.6395(6) 1.0335(6) 0.0560(7) 0.099(3) Uani 0.25 1 d PDU . 1
O1B O 0.5534(8) 1.0081(6) 0.1442(7) 0.106(4) Uani 0.22 1 d PDU B 2
O2B O 0.6482(6) 1.0330(6) 0.0000 0.114(3) Uani 0.44 2 d SPDU A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 '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
N1 C1 Mo1 178.2(4) . . ?
N1 C2 C7 118.4(4) . . ?
N1 C2 C3 119.0(4) . . ?
C7 C2 C3 122.5(3) . . ?
C4 C3 C2 117.4(4) . . ?
C4 C3 C15 121.5(4) . . ?
C2 C3 C15 121.1(3) . . ?
C3 C4 C5 121.9(4) . . ?
C4 C5 C6 119.6(4) . . ?
C7 C6 C5 121.1(4) . . ?
C6 C7 C2 117.5(4) . . ?
C6 C7 C8 122.3(4) . . ?
C2 C7 C8 120.2(3) . . ?
C9 C8 C9 119.7(4) 12 . ?
C9 C8 C7 120.1(2) 12 . ?
C9 C8 C7 120.1(2) . . ?
C10 C9 C8 118.8(4) . . ?
C10 C9 C12 119.4(4) . . ?
C8 C9 C12 121.8(3) . . ?
C11 C10 C9 121.8(4) . . ?
C10 C11 C10 118.9(5) 12 . ?
C9 C12 C14 111.9(4) . . ?
C9 C12 C13 111.9(4) . . ?
C14 C12 C13 112.1(4) . . ?
C16 C15 C16 120.5(5) . 12 ?
C16 C15 C3 119.8(2) . . ?
C16 C15 C3 119.8(2) 12 . ?
C17 C16 C15 118.5(4) . . ?
C17 C16 C19 119.4(4) . . ?
C15 C16 C19 122.0(3) . . ?
C18 C17 C16 120.9(6) . . ?
C17 C18 C17 120.7(7) . 12 ?
C21 C19 C16 112.0(5) . . ?
C21 C19 C20 109.0(4) . . ?
C16 C19 C20 111.8(4) . . ?
O2A C2OA C2OA 101.4(12) . 12 ?
O2A C2OA Mo1 165.5(17) . . ?
C2OA C2OA Mo1 64.2(5) 12 . ?
O1B C1OB C1OB 101.4(14) . 4_675 ?
O1B C1OB Mo1 164.8(18) . . ?
C1OB C1OB Mo1 63.4(5) 4_675 . ?
O2B C2OB Mo1 179.5(11) . . ?
C1S C2S C1S 180.000(2) 14_465 . ?
C1OB Mo1 C1OB 53.2(11) 12 9_675 ?
C1OB Mo1 C1OB 126.8(11) 12 . ?
C1OB Mo1 C1OB 180.000(2) 9_675 . ?
C1OB Mo1 C1OB 180.000(3) 12 4_675 ?
C1OB Mo1 C1OB 126.8(11) 9_675 4_675 ?
C1OB Mo1 C1OB 53.2(11) . 4_675 ?
C1OB Mo1 C2OB 63.4(5) 12 . ?
C1OB Mo1 C2OB 116.6(5) 9_675 . ?
C1OB Mo1 C2OB 63.4(5) . . ?
C1OB Mo1 C2OB 116.6(5) 4_675 . ?
C1OB Mo1 C2OB 116.6(5) 12 9_675 ?
C1OB Mo1 C2OB 63.4(5) 9_675 9_675 ?
C1OB Mo1 C2OB 116.6(5) . 9_675 ?
C1OB Mo1 C2OB 63.4(5) 4_675 9_675 ?
C2OB Mo1 C2OB 180.000(1) . 9_675 ?
C1OB Mo1 C2OA 89.3(9) 12 . ?
C1OB Mo1 C2OA 142.3(7) 9_675 . ?
C1OB Mo1 C2OA 37.7(7) . . ?
C1OB Mo1 C2OA 90.7(9) 4_675 . ?
C2OB Mo1 C2OA 25.9(5) . . ?
C2OB Mo1 C2OA 154.1(5) 9_675 . ?
C1OB Mo1 C2OA 90.7(9) 12 9_675 ?
C1OB Mo1 C2OA 37.7(7) 9_675 9_675 ?
C1OB Mo1 C2OA 142.3(7) . 9_675 ?
C1OB Mo1 C2OA 89.3(9) 4_675 9_675 ?
C2OB Mo1 C2OA 154.1(5) . 9_675 ?
C2OB Mo1 C2OA 25.9(5) 9_675 9_675 ?
C2OA Mo1 C2OA 180.000(2) . 9_675 ?
C1OB Mo1 C2OA 37.7(7) 12 12 ?
C1OB Mo1 C2OA 90.7(9) 9_675 12 ?
C1OB Mo1 C2OA 89.3(9) . 12 ?
C1OB Mo1 C2OA 142.3(7) 4_675 12 ?
C2OB Mo1 C2OA 25.9(5) . 12 ?
C2OB Mo1 C2OA 154.1(5) 9_675 12 ?
C2OA Mo1 C2OA 51.6(11) . 12 ?
C2OA Mo1 C2OA 128.4(11) 9_675 12 ?
C1OB Mo1 C2OA 142.3(7) 12 4_675 ?
C1OB Mo1 C2OA 89.3(9) 9_675 4_675 ?
C1OB Mo1 C2OA 90.7(9) . 4_675 ?
C1OB Mo1 C2OA 37.7(7) 4_675 4_675 ?
C2OB Mo1 C2OA 154.1(5) . 4_675 ?
C2OB Mo1 C2OA 25.9(5) 9_675 4_675 ?
C2OA Mo1 C2OA 128.4(11) . 4_675 ?
C2OA Mo1 C2OA 51.6(11) 9_675 4_675 ?
C2OA Mo1 C2OA 180.000(1) 12 4_675 ?
C1OB Mo1 C1OA 153.4(5) 12 . ?
C1OB Mo1 C1OA 153.4(5) 9_675 . ?
C1OB Mo1 C1OA 26.6(5) . . ?
C1OB Mo1 C1OA 26.6(5) 4_675 . ?
C2OB Mo1 C1OA 90.000(1) . . ?
C2OB Mo1 C1OA 90.000(1) 9_675 . ?
C2OA Mo1 C1OA 64.2(5) . . ?
C2OA Mo1 C1OA 115.8(5) 9_675 . ?
C2OA Mo1 C1OA 115.8(5) 12 . ?
C2OA Mo1 C1OA 64.2(5) 4_675 . ?
C1 N1 C2 176.1(5) . . ?
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
C1 N1 1.137(6) . ?
C1 Mo1 2.083(5) . ?
C2 N1 1.386(5) . ?
C2 C7 1.400(6) . ?
C2 C3 1.400(6) . ?
C3 C4 1.365(6) . ?
C3 C15 1.492(6) . ?
C4 C5 1.370(7) . ?
C5 C6 1.401(7) . ?
C6 C7 1.363(6) . ?
C7 C8 1.490(6) . ?
C8 C9 1.396(4) 12 ?
C8 C9 1.396(4) . ?
C9 C10 1.386(5) . ?
C9 C12 1.498(5) . ?
C10 C11 1.365(5) . ?
C11 C10 1.365(5) 12 ?
C12 C14 1.504(6) . ?
C12 C13 1.524(7) . ?
C15 C16 1.400(4) . ?
C15 C16 1.400(4) 12 ?
C16 C17 1.384(6) . ?
C16 C19 1.506(7) . ?
C17 C18 1.365(6) . ?
C18 C17 1.365(6) 12 ?
C19 C21 1.505(7) . ?
C19 C20 1.547(8) . ?
C1OA Mo1 2.077(15) . ?
C2OA O2A 1.159(14) . ?
C2OA C2OA 1.77(4) 12 ?
C2OA Mo1 2.039(12) . ?
C1OB O1B 1.097(14) . ?
C1OB C1OB 1.80(4) 4_675 ?
C1OB Mo1 2.012(13) . ?
C2OB O2B 1.107(13) . ?
C2OB Mo1 2.037(10) . ?
C1S C2S 1.683(15) . ?
C2S C1S 1.683(15) 14_465 ?
Mo1 C1OB 2.012(13) 12 ?
Mo1 C1OB 2.012(13) 9_675 ?
Mo1 C1OB 2.012(13) 4_675 ?
Mo1 C2OB 2.037(10) 9_675 ?
Mo1 C2OA 2.039(12) 9_675 ?
Mo1 C2OA 2.039(12) 12 ?
Mo1 C2OA 2.039(12) 4_675 ?
