#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:40:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178819 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/73/4107337.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_4107337
loop_
_publ_author_name
'Soumya Sarkar'
'Adam R. Carlson'
'Melanie K. Veige'
'Joseph M. Falkowski'
'Khalil A. Abboud'
'Adam S. Veige'
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of a d2, Mo(IV) Complex
 Supported by a New OCO-Trianionic Pincer Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1116
_journal_page_last               1117
_journal_paper_doi               10.1021/ja074901k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C42 H53 Cl Mo N2 O2'
_chemical_formula_weight         749.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   10.4875(8)
_cell_length_b                   17.2088(13)
_cell_length_c                   21.1554(15)
_cell_measurement_reflns_used    186
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3818.1(5)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24328
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0263
_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)+(0.0379P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                3320
_reflns_number_total             4392
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja074901k-file001.cif
_cod_data_source_block           ac12
_cod_database_code               4107337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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 0.026259(11) 0.7500 0.01800(7) Uani 1 2 d S
Cl1 Cl 0.0000 0.17054(3) 0.7500 0.02571(14) Uani 1 2 d S
O1 O -0.09328(10) 0.01185(6) 0.82834(5) 0.0206(3) Uani 1 1 d .
N1 N 0.16666(15) 0.03652(9) 0.81451(7) 0.0264(3) Uani 1 1 d .
H1 H 0.140(2) 0.0709(14) 0.8379(11) 0.060(8) Uiso 1 1 d .
C1 C 0.0000 -0.09693(12) 0.7500 0.0188(5) Uani 1 2 d S
C2 C -0.10453(16) -0.13941(9) 0.77538(8) 0.0218(4) Uani 1 1 d .
C3 C -0.10275(18) -0.22065(10) 0.77421(8) 0.0280(4) Uani 1 1 d .
H3A H -0.1736 -0.2488 0.7904 0.034 Uiso 1 1 calc R
C4 C 0.0000 -0.26049(15) 0.7500 0.0308(6) Uani 1 2 d S
H4A H 0.0000 -0.3157 0.7500 0.037 Uiso 1 2 calc SR
C5 C -0.21537(17) -0.10133(10) 0.80672(7) 0.0226(4) Uani 1 1 d .
C6 C -0.20033(16) -0.03028(9) 0.83880(7) 0.0204(3) Uani 1 1 d .
C7 C -0.29290(16) -0.00262(10) 0.88168(8) 0.0224(4) Uani 1 1 d .
C8 C -0.40917(17) -0.04177(11) 0.88270(9) 0.0303(4) Uani 1 1 d .
H8A H -0.4751 -0.0234 0.9096 0.036 Uiso 1 1 calc R
C9 C -0.43150(19) -0.10670(12) 0.84567(9) 0.0356(5) Uani 1 1 d .
H9A H -0.5137 -0.1298 0.8451 0.043 Uiso 1 1 calc R
C10 C -0.33470(17) -0.13791(11) 0.80960(8) 0.0289(4) Uani 1 1 d .
H10A H -0.3490 -0.1845 0.7866 0.035 Uiso 1 1 calc R
C11 C -0.26595(16) 0.06719(10) 0.92534(7) 0.0250(4) Uani 1 1 d .
C12 C -0.37033(19) 0.07660(13) 0.97566(9) 0.0372(5) Uani 1 1 d .
H12C H -0.4526 0.0853 0.9549 0.056 Uiso 1 1 calc R
H12B H -0.3501 0.1212 1.0027 0.056 Uiso 1 1 calc R
H12A H -0.3748 0.0294 1.0015 0.056 Uiso 1 1 calc R
C13 C -0.2607(2) 0.14227(11) 0.88666(9) 0.0368(5) Uani 1 1 d .
H13C H -0.1945 0.1377 0.8542 0.055 Uiso 1 1 calc R
H13B H -0.2406 0.1860 0.9146 0.055 Uiso 1 1 calc R
H13A H -0.3434 0.1512 0.8664 0.055 Uiso 1 1 calc R
C14 C -0.13974(18) 0.05471(12) 0.96124(9) 0.0330(4) Uani 1 1 d .
H14C H -0.0700 0.0484 0.9309 0.050 Uiso 1 1 calc R
H14B H -0.1463 0.0080 0.9875 0.050 Uiso 1 1 calc R
H14A H -0.1227 0.0998 0.9882 0.050 Uiso 1 1 calc R
C15 C 0.28671(17) 0.06811(12) 0.78776(9) 0.0327(4) Uani 1 1 d .
H15C H 0.3519 0.0703 0.8209 0.049 Uiso 1 1 calc R
H15B H 0.2714 0.1205 0.7713 0.049 Uiso 1 1 calc R
H15A H 0.3162 0.0344 0.7534 0.049 Uiso 1 1 calc R
C16 C 0.1933(2) -0.02872(11) 0.85756(9) 0.0352(5) Uani 1 1 d .
H16C H 0.2681 -0.0164 0.8835 0.053 Uiso 1 1 calc R
H16B H 0.2102 -0.0757 0.8328 0.053 Uiso 1 1 calc R
H16A H 0.1195 -0.0375 0.8850 0.053 Uiso 1 1 calc R
C17 C 0.1328(2) 0.20482(13) 0.91419(11) 0.0489(6) Uani 1 1 d .
H17A H 0.0485 0.1988 0.8985 0.059 Uiso 1 1 calc R
C18 C 0.1656(3) 0.17314(13) 0.97139(12) 0.0548(6) Uani 1 1 d .
H18A H 0.1042 0.1446 0.9949 0.066 Uiso 1 1 calc R
C19 C 0.2857(3) 0.18230(14) 0.99469(12) 0.0656(8) Uani 1 1 d .
H19A H 0.3086 0.1605 1.0343 0.079 Uiso 1 1 calc R
C20 C 0.3752(2) 0.22448(16) 0.95925(16) 0.0697(9) Uani 1 1 d .
H20A H 0.4593 0.2318 0.9748 0.084 Uiso 1 1 calc R
C21 C 0.3401(3) 0.25511(14) 0.90186(13) 0.0598(7) Uani 1 1 d .
H21A H 0.4000 0.2837 0.8775 0.072 Uiso 1 1 calc R
C22 C 0.2200(2) 0.24451(13) 0.88020(11) 0.0519(6) Uani 1 1 d .
H22A H 0.1966 0.2654 0.8403 0.062 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
O1 Mo1 O1 165.32(6) 3_556 .
O1 Mo1 C1 82.66(3) 3_556 .
O1 Mo1 C1 82.66(3) . .
O1 Mo1 N1 97.93(5) 3_556 .
O1 Mo1 N1 83.24(5) . .
C1 Mo1 N1 94.55(4) . .
O1 Mo1 N1 83.24(5) 3_556 3_556
O1 Mo1 N1 97.93(5) . 3_556
C1 Mo1 N1 94.55(4) . 3_556
N1 Mo1 N1 170.90(8) . 3_556
O1 Mo1 Cl1 97.34(3) 3_556 .
O1 Mo1 Cl1 97.34(3) . .
C1 Mo1 Cl1 180.0 . .
N1 Mo1 Cl1 85.45(4) . .
N1 Mo1 Cl1 85.45(4) 3_556 .
C6 O1 Mo1 128.73(10) . .
C16 N1 C15 110.73(15) . .
C16 N1 Mo1 117.92(12) . .
C15 N1 Mo1 117.51(11) . .
C16 N1 H1 103.9(17) . .
C15 N1 H1 104.5(17) . .
Mo1 N1 H1 99.5(17) . .
C2 C1 C2 118.2(2) . 3_556
C2 C1 Mo1 120.92(10) . .
C2 C1 Mo1 120.92(10) 3_556 .
C3 C2 C1 119.78(16) . .
C3 C2 C5 117.26(15) . .
C1 C2 C5 122.89(15) . .
C4 C3 C2 121.01(18) . .
C4 C3 H3A 119.5 . .
C2 C3 H3A 119.5 . .
C3 C4 C3 120.2(2) . 3_556
C3 C4 H4A 119.9 . .
C3 C4 H4A 119.9 3_556 .
C10 C5 C6 117.98(16) . .
C10 C5 C2 121.21(16) . .
C6 C5 C2 120.61(15) . .
O1 C6 C5 118.63(14) . .
O1 C6 C7 119.64(14) . .
C5 C6 C7 121.73(15) . .
C8 C7 C6 116.67(16) . .
C8 C7 C11 121.88(15) . .
C6 C7 C11 121.45(15) . .
C9 C8 C7 121.97(17) . .
C9 C8 H8A 119.0 . .
C7 C8 H8A 119.0 . .
C10 C9 C8 120.19(17) . .
C10 C9 H9A 119.9 . .
C8 C9 H9A 119.9 . .
C9 C10 C5 120.42(17) . .
C9 C10 H10A 119.8 . .
C5 C10 H10A 119.8 . .
C13 C11 C12 107.91(15) . .
C13 C11 C14 110.49(15) . .
C12 C11 C14 106.57(14) . .
C13 C11 C7 110.14(14) . .
C12 C11 C7 111.52(15) . .
C14 C11 C7 110.13(14) . .
C11 C12 H12C 109.5 . .
C11 C12 H12B 109.5 . .
H12C C12 H12B 109.5 . .
C11 C12 H12A 109.5 . .
H12C C12 H12A 109.5 . .
H12B C12 H12A 109.5 . .
C11 C13 H13C 109.5 . .
C11 C13 H13B 109.5 . .
H13C C13 H13B 109.5 . .
C11 C13 H13A 109.5 . .
H13C C13 H13A 109.5 . .
H13B C13 H13A 109.5 . .
C11 C14 H14C 109.5 . .
C11 C14 H14B 109.5 . .
H14C C14 H14B 109.5 . .
C11 C14 H14A 109.5 . .
H14C C14 H14A 109.5 . .
H14B C14 H14A 109.5 . .
N1 C15 H15C 109.5 . .
N1 C15 H15B 109.5 . .
H15C C15 H15B 109.5 . .
N1 C15 H15A 109.5 . .
H15C C15 H15A 109.5 . .
H15B C15 H15A 109.5 . .
N1 C16 H16C 109.5 . .
N1 C16 H16B 109.5 . .
H16C C16 H16B 109.5 . .
N1 C16 H16A 109.5 . .
H16C C16 H16A 109.5 . .
H16B C16 H16A 109.5 . .
C22 C17 C18 120.1(2) . .
C22 C17 H17A 119.9 . .
C18 C17 H17A 119.9 . .
C19 C18 C17 120.4(2) . .
C19 C18 H18A 119.8 . .
C17 C18 H18A 119.8 . .
C18 C19 C20 119.0(2) . .
C18 C19 H19A 120.5 . .
C20 C19 H19A 120.5 . .
C21 C20 C19 119.4(2) . .
C21 C20 H20A 120.3 . .
C19 C20 H20A 120.3 . .
C22 C21 C20 119.8(2) . .
C22 C21 H21A 120.1 . .
C20 C21 H21A 120.1 . .
C17 C22 C21 121.3(2) . .
C17 C22 H22A 119.4 . .
C21 C22 H22A 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.9405(11) 3_556
Mo1 O1 1.9405(11) .
Mo1 C1 2.120(2) .
Mo1 N1 2.2245(16) .
Mo1 N1 2.2245(16) 3_556
Mo1 Cl1 2.4829(6) .
O1 C6 1.3547(19) .
N1 C16 1.473(2) .
N1 C15 1.484(2) .
N1 H1 0.82(2) .
C1 C2 1.423(2) .
C1 C2 1.423(2) 3_556
C2 C3 1.398(2) .
C2 C5 1.490(2) .
C3 C4 1.376(2) .
C3 H3A 0.9500 .
C4 C3 1.376(2) 3_556
C4 H4A 0.9500 .
C5 C10 1.402(2) .
C5 C6 1.407(2) .
C6 C7 1.411(2) .
C7 C8 1.393(2) .
C7 C11 1.541(2) .
C8 C9 1.385(3) .
C8 H8A 0.9500 .
C9 C10 1.379(3) .
C9 H9A 0.9500 .
C10 H10A 0.9500 .
C11 C13 1.530(2) .
C11 C12 1.536(2) .
C11 C14 1.541(2) .
C12 H12C 0.9800 .
C12 H12B 0.9800 .
C12 H12A 0.9800 .
C13 H13C 0.9800 .
C13 H13B 0.9800 .
C13 H13A 0.9800 .
C14 H14C 0.9800 .
C14 H14B 0.9800 .
C14 H14A 0.9800 .
C15 H15C 0.9800 .
C15 H15B 0.9800 .
C15 H15A 0.9800 .
C16 H16C 0.9800 .
C16 H16B 0.9800 .
C16 H16A 0.9800 .
C17 C22 1.349(3) .
C17 C18 1.371(3) .
C17 H17A 0.9500 .
C18 C19 1.362(4) .
C18 H18A 0.9500 .
C19 C20 1.404(4) .
C19 H19A 0.9500 .
C20 C21 1.374(4) .
C20 H20A 0.9500 .
C21 C22 1.353(3) .
C21 H21A 0.9500 .
C22 H22A 0.9500 .
