#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:34:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179067 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/29/4302946.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_4302946
loop_
_publ_author_name
'Patrick Achord'
'Etsuko Fujita'
'James T. Muckerman'
'Brian Scott'
'George C. Fortman'
'Manuel Temprado'
'Xiaochen Cai'
'Burjor Captain'
'Derek Isrow'
'John J. Weir'
'James Eric McDonough'
'Carl D. Hoff'
_publ_section_title
;
Experimental and Computational Studies of Binding of Dinitrogen, Nitriles,
Azides, Diazoalkanes, Pyridine, and Pyrazines to M(PR3)2(CO)3 (M = Mo, W; R
= Me,iPr).
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7891
_journal_page_last               7904
_journal_paper_doi               10.1021/ic900764e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C24 H48 N2 O3 P2 W'
_chemical_formula_weight         658.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 107.7430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1406(6)
_cell_length_b                   11.4630(5)
_cell_length_c                   20.0187(11)
_cell_measurement_temperature    120(1)
_cell_volume                     2872.0(2)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11153
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.159
_exptl_absorpt_correction_T_max  0.7885
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.918
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.604
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.604
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                3291
_reflns_number_total             3482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900764e_si_002_4.cif
_cod_data_source_block           WkNCNMe2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302946
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
W1 W 0.5000 0.263002(14) 0.7500 0.01125(8) Uani 1 2 d S . .
P1 P 0.53722(8) 0.24830(7) 0.63532(5) 0.01516(19) Uani 1 1 d . . .
O1 O 0.5000 0.5340(3) 0.7500 0.0257(9) Uani 1 2 d S . .
O2 O 0.2553(2) 0.3090(3) 0.67184(16) 0.0405(8) Uani 1 1 d . . .
C1 C 0.5322(4) 0.3876(3) 0.5869(2) 0.0302(10) Uani 1 1 d . . .
H1 H 0.5423 0.3690 0.5416 0.036 Uiso 1 1 calc R . .
C2 C 0.6221(5) 0.4726(5) 0.6257(3) 0.0623(18) Uani 1 1 d . . .
H2A H 0.6902 0.4351 0.6337 0.093 Uiso 1 1 calc R . .
H2B H 0.6129 0.4943 0.6698 0.093 Uiso 1 1 calc R . .
H2C H 0.6192 0.5411 0.5975 0.093 Uiso 1 1 calc R . .
C3 C 0.4229(5) 0.4445(4) 0.5725(2) 0.0517(15) Uani 1 1 d . . .
H3A H 0.3684 0.3903 0.5484 0.077 Uiso 1 1 calc R . .
H3B H 0.4193 0.5126 0.5440 0.077 Uiso 1 1 calc R . .
H3C H 0.4120 0.4665 0.6161 0.077 Uiso 1 1 calc R . .
C4 C 0.4531(5) 0.1475(5) 0.5687(2) 0.0565(16) Uani 1 1 d . . .
H4 H 0.4977 0.0772 0.5773 0.068 Uiso 1 1 calc R . .
C5 C 0.4409(4) 0.1704(4) 0.4913(2) 0.0364(10) Uani 1 1 d . . .
H5A H 0.5074 0.1982 0.4869 0.055 Uiso 1 1 calc R . .
H5B H 0.3864 0.2281 0.4733 0.055 Uiso 1 1 calc R . .
H5C H 0.4212 0.0994 0.4652 0.055 Uiso 1 1 calc R . .
C6 C 0.3571(4) 0.1037(5) 0.5786(3) 0.0517(15) Uani 1 1 d . . .
H6A H 0.3683 0.0897 0.6276 0.078 Uiso 1 1 calc R . .
H6B H 0.3374 0.0320 0.5531 0.078 Uiso 1 1 calc R . .
H6C H 0.3009 0.1598 0.5618 0.078 Uiso 1 1 calc R . .
C7 C 0.6756(5) 0.1983(7) 0.6437(3) 0.076(2) Uani 1 1 d . . .
H7 H 0.7192 0.2622 0.6702 0.092 Uiso 1 1 calc R . .
C8 C 0.7149(4) 0.1009(5) 0.6875(3) 0.0479(14) Uani 1 1 d . . .
H8A H 0.6944 0.1074 0.7294 0.072 Uiso 1 1 calc R . .
H8B H 0.7914 0.0987 0.6996 0.072 Uiso 1 1 calc R . .
H8C H 0.6856 0.0306 0.6631 0.072 Uiso 1 1 calc R . .
C9 C 0.7079(4) 0.1971(6) 0.5762(3) 0.0555(15) Uani 1 1 d . . .
H9A H 0.6799 0.2652 0.5488 0.083 Uiso 1 1 calc R . .
H9B H 0.6796 0.1284 0.5495 0.083 Uiso 1 1 calc R . .
H9C H 0.7844 0.1969 0.5879 0.083 Uiso 1 1 calc R . .
C10 C 0.5000 0.4312(4) 0.7500 0.0180(10) Uani 1 2 d S . .
C11 C 0.3437(3) 0.2838(3) 0.7005(2) 0.0216(7) Uani 1 1 d . . .
C12 C 0.5000 -0.0286(5) 0.7500 0.0358(16) Uani 1 2 d S . .
C13 C 0.4874(4) -0.2053(4) 0.8091(2) 0.0358(11) Uani 1 1 d . . .
H13A H 0.4889 -0.2878 0.8012 0.054 Uiso 1 1 calc R . .
H13B H 0.4203 -0.1844 0.8155 0.054 Uiso 1 1 calc R . .
H13C H 0.5445 -0.1847 0.8502 0.054 Uiso 1 1 calc R . .
N1 N 0.5000 0.0718(4) 0.7500 0.0256(10) Uani 1 2 d S . .
N2 N 0.5000 -0.1444(4) 0.7500 0.074(3) Uani 1 2 d S . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C10 W1 C11 83.17(11) . 2_656 ?
C10 W1 C11 83.17(11) . . ?
C11 W1 C11 166.3(2) 2_656 . ?
C10 W1 N1 180.000(2) . . ?
C11 W1 N1 96.83(11) 2_656 . ?
C11 W1 N1 96.83(11) . . ?
C10 W1 P1 93.873(19) . 2_656 ?
C11 W1 P1 90.66(11) 2_656 2_656 ?
C11 W1 P1 90.26(11) . 2_656 ?
N1 W1 P1 86.127(19) . 2_656 ?
C10 W1 P1 93.873(19) . . ?
C11 W1 P1 90.26(11) 2_656 . ?
C11 W1 P1 90.66(11) . . ?
N1 W1 P1 86.127(19) . . ?
P1 W1 P1 172.25(4) 2_656 . ?
C4 P1 C1 104.0(2) . . ?
C4 P1 C7 103.0(3) . . ?
C1 P1 C7 100.9(3) . . ?
C4 P1 W1 117.58(15) . . ?
C1 P1 W1 115.86(13) . . ?
C7 P1 W1 113.42(18) . . ?
C3 C1 C2 111.0(4) . . ?
C3 C1 P1 110.4(3) . . ?
C2 C1 P1 112.3(3) . . ?
C6 C4 C5 112.1(4) . . ?
C6 C4 P1 118.6(4) . . ?
C5 C4 P1 118.5(3) . . ?
C8 C7 C9 113.0(5) . . ?
C8 C7 P1 117.4(4) . . ?
C9 C7 P1 116.6(4) . . ?
O1 C10 W1 180.000(1) . . ?
O2 C11 W1 172.4(4) . . ?
N1 C12 N2 180.000(3) . . ?
C12 N1 W1 180.000(1) . . ?
C12 N2 C13 119.3(2) . 2_656 ?
C12 N2 C13 119.3(2) . . ?
C13 N2 C13 121.4(5) 2_656 . ?
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
W1 C10 1.928(5) . ?
W1 C11 2.004(4) 2_656 ?
W1 C11 2.004(4) . ?
W1 N1 2.192(5) . ?
W1 P1 2.4943(10) 2_656 ?
W1 P1 2.4944(10) . ?
P1 C4 1.854(5) . ?
P1 C1 1.858(4) . ?
P1 C7 1.865(5) . ?
O1 C10 1.178(6) . ?
O2 C11 1.165(5) . ?
C1 C3 1.524(6) . ?
C1 C2 1.545(6) . ?
C4 C6 1.427(6) . ?
C4 C5 1.531(6) . ?
C7 C8 1.417(7) . ?
C7 C9 1.535(6) . ?
C12 N1 1.151(7) . ?
C12 N2 1.328(7) . ?
C13 N2 1.425(5) . ?
N2 C13 1.425(5) 2_656 ?
