#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:39:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180048 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/42/7034242.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_7034242
loop_
_publ_author_name
'Chakraborty, Subrata'
'Blacque, Olivier'
'Berke, Heinz'
_publ_section_title
;
 Ligand assisted carbon dioxide activation and hydrogenation using
 molybdenum and tungsten amides.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6560
_journal_page_last               6570
_journal_paper_doi               10.1039/c5dt00278h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C18 H36 N2 O4 P2 W'
_chemical_formula_sum            'C18 H36 N2 O4 P2 W'
_chemical_formula_weight         590.28
_chemical_name_systematic
'(bis{2-[bis(1-methylethyl)phosphanyl-κP]ethyl}carbamato-κ²N,O)(carbonyl)(nitrosyl)tungsten '
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-09-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.979(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8847(1)
_cell_length_b                   26.3644(4)
_cell_length_c                   11.5872(2)
_cell_measurement_reflns_used    27135
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.67
_cell_measurement_theta_min      2.70
_cell_volume                     2303.70(7)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) 
;
_computing_publication_material
; 
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37089
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.178
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.35.11 (Agilent, 2011).
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid (1995).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.657
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0093P)²+2.1311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0403
_reflns_number_gt                5574
_reflns_number_total             5720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00278h2.cif
_cod_data_source_block           2b(trans)
_cod_depositor_comments
'Adding full bibliography for 7034242--7034245.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7034242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.9429(3) 0.15311(10) 0.2801(2) 0.0250(5) Uani 1 1 d .
C2 C 0.5948(3) 0.02971(9) 0.2558(2) 0.0214(5) Uani 1 1 d .
C3 C 0.4417(3) 0.18271(10) -0.0234(2) 0.0260(5) Uani 1 1 d .
H3 H 0.5273 0.2105 -0.0138 0.031 Uiso 1 1 calc R
C4 C 0.3014(4) 0.19968(12) 0.0358(3) 0.0350(7) Uani 1 1 d .
H4A H 0.2511 0.2314 0.0015 0.052 Uiso 1 1 calc R
H4B H 0.3553 0.2038 0.1210 0.052 Uiso 1 1 calc R
H4C H 0.2097 0.1745 0.0222 0.052 Uiso 1 1 calc R
C5 C 0.3563(4) 0.17531(13) -0.1588(3) 0.0413(8) Uani 1 1 d .
H5A H 0.2703 0.1485 -0.1716 0.062 Uiso 1 1 calc R
H5B H 0.4460 0.1666 -0.1963 0.062 Uiso 1 1 calc R
H5C H 0.2989 0.2062 -0.1934 0.062 Uiso 1 1 calc R
C6 C 0.7011(3) 0.10688(11) -0.0462(2) 0.0257(5) Uani 1 1 d .
H6 H 0.6223 0.0983 -0.1262 0.031 Uiso 1 1 calc R
C7 C 0.8193(4) 0.15142(12) -0.0580(2) 0.0321(6) Uani 1 1 d .
H7A H 0.8839 0.1633 0.0209 0.048 Uiso 1 1 calc R
H7B H 0.7469 0.1784 -0.1021 0.048 Uiso 1 1 calc R
H7C H 0.9011 0.1405 -0.1001 0.048 Uiso 1 1 calc R
C8 C 0.8151(4) 0.06071(12) 0.0056(3) 0.0342(6) Uani 1 1 d .
H8A H 0.8827 0.0510 -0.0476 0.051 Uiso 1 1 calc R
H8B H 0.7399 0.0331 0.0135 0.051 Uiso 1 1 calc R
H8C H 0.8942 0.0690 0.0834 0.051 Uiso 1 1 calc R
C9 C 0.3947(3) 0.07696(10) 0.0348(2) 0.0238(5) Uani 1 1 d .
H9A H 0.2968 0.0840 -0.0365 0.029 Uiso 1 1 calc R
H9B H 0.4443 0.0443 0.0238 0.029 Uiso 1 1 calc R
C10 C 0.3264(3) 0.07489(10) 0.1451(2) 0.0228(5) Uani 1 1 d .
H10A H 0.2512 0.1040 0.1447 0.027 Uiso 1 1 calc R
H10B H 0.2555 0.0445 0.1415 0.027 Uiso 1 1 calc R
C11 C 0.4092(3) 0.07084(10) 0.3662(2) 0.0231(5) Uani 1 1 d .
H11A H 0.3278 0.0425 0.3559 0.028 Uiso 1 1 calc R
H11B H 0.3450 0.1015 0.3731 0.028 Uiso 1 1 calc R
C12 C 0.5624(3) 0.06339(10) 0.4811(2) 0.0236(5) Uani 1 1 d .
H12A H 0.6054 0.0288 0.4838 0.028 Uiso 1 1 calc R
H12B H 0.5198 0.0685 0.5507 0.028 Uiso 1 1 calc R
C13 C 0.9381(3) 0.06785(11) 0.5705(2) 0.0270(6) Uani 1 1 d .
H13 H 0.9212 0.0352 0.5283 0.032 Uiso 1 1 calc R
C14 C 0.9452(4) 0.05604(12) 0.7007(2) 0.0338(6) Uani 1 1 d .
H14A H 1.0299 0.0295 0.7312 0.051 Uiso 1 1 calc R
H14B H 0.8302 0.0452 0.7036 0.051 Uiso 1 1 calc R
H14C H 0.9799 0.0859 0.7492 0.051 Uiso 1 1 calc R
C15 C 1.1145(4) 0.08829(14) 0.5620(3) 0.0432(8) Uani 1 1 d .
H15A H 1.1366 0.1209 0.6003 0.065 Uiso 1 1 calc R
H15B H 1.1103 0.0916 0.4787 0.065 Uiso 1 1 calc R
H15C H 1.2078 0.0653 0.6016 0.065 Uiso 1 1 calc R
C16 C 0.7199(4) 0.15804(10) 0.5927(2) 0.0257(5) Uani 1 1 d .
H16 H 0.7403 0.1429 0.6728 0.031 Uiso 1 1 calc R
C17 C 0.8547(4) 0.20073(12) 0.6034(3) 0.0403(7) Uani 1 1 d .
H17A H 0.8437 0.2145 0.5249 0.060 Uiso 1 1 calc R
H17B H 0.9723 0.1876 0.6373 0.060 Uiso 1 1 calc R
H17C H 0.8328 0.2269 0.6549 0.060 Uiso 1 1 calc R
C18 C 0.5308(4) 0.17906(11) 0.5535(3) 0.0316(6) Uani 1 1 d .
H18A H 0.5196 0.2052 0.6084 0.047 Uiso 1 1 calc R
H18B H 0.4485 0.1523 0.5539 0.047 Uiso 1 1 calc R
H18C H 0.5055 0.1928 0.4736 0.047 Uiso 1 1 calc R
N1 N 0.6421(3) 0.19345(8) 0.28873(17) 0.0205(4) Uani 1 1 d .
N2 N 0.4771(3) 0.07465(8) 0.25918(17) 0.0181(4) Uani 1 1 d .
O1 O 1.0838(3) 0.16676(9) 0.2828(2) 0.0438(6) Uani 1 1 d .
O2 O 0.6004(3) 0.23680(7) 0.30062(17) 0.0356(5) Uani 1 1 d .
O3 O 0.7506(2) 0.04650(7) 0.26377(16) 0.0237(4) Uani 1 1 d .
O4 O 0.5375(3) -0.01304(7) 0.24741(18) 0.0330(4) Uani 1 1 d .
P1 P 0.56579(8) 0.12643(2) 0.05210(5) 0.01864(12) Uani 1 1 d .
P2 P 0.74744(8) 0.10777(2) 0.48901(5) 0.01853(12) Uani 1 1 d .
W1 W 0.704076(12) 0.129037(3) 0.273888(8) 0.01562(3) Uani 1 1 d .
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
O1 C1 W1 179.1(3)
O4 C2 O3 130.9(2)
O4 C2 N2 121.0(2)
O3 C2 N2 108.0(2)
C5 C3 C4 109.8(2)
C5 C3 P1 113.4(2)
C4 C3 P1 111.96(18)
C5 C3 H3 107.1
C4 C3 H3 107.1
P1 C3 H3 107.1
C3 C4 H4A 109.5
C3 C4 H4B 109.5
H4A C4 H4B 109.5
C3 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
C3 C5 H5A 109.5
C3 C5 H5B 109.5
H5A C5 H5B 109.5
C3 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
C8 C6 C7 110.1(2)
C8 C6 P1 111.07(18)
C7 C6 P1 108.51(19)
C8 C6 H6 109.1
C7 C6 H6 109.1
P1 C6 H6 109.1
C6 C7 H7A 109.5
C6 C7 H7B 109.5
H7A C7 H7B 109.5
C6 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
C6 C8 H8A 109.5
C6 C8 H8B 109.5
H8A C8 H8B 109.5
C6 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
C10 C9 P1 111.12(17)
C10 C9 H9A 109.4
P1 C9 H9A 109.4
C10 C9 H9B 109.4
P1 C9 H9B 109.4
H9A C9 H9B 108.0
N2 C10 C9 110.86(19)
N2 C10 H10A 109.5
C9 C10 H10A 109.5
N2 C10 H10B 109.5
C9 C10 H10B 109.5
H10A C10 H10B 108.1
N2 C11 C12 110.4(2)
N2 C11 H11A 109.6
C12 C11 H11A 109.6
N2 C11 H11B 109.6
C12 C11 H11B 109.6
H11A C11 H11B 108.1
C11 C12 P2 111.93(17)
C11 C12 H12A 109.2
P2 C12 H12A 109.2
C11 C12 H12B 109.2
P2 C12 H12B 109.2
H12A C12 H12B 107.9
C15 C13 C14 111.5(2)
C15 C13 P2 112.8(2)
C14 C13 P2 114.18(19)
C15 C13 H13 105.9
C14 C13 H13 105.9
P2 C13 H13 105.9
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
C13 C15 H15A 109.5
C13 C15 H15B 109.5
H15A C15 H15B 109.5
C13 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
C17 C16 C18 110.6(2)
C17 C16 P2 111.79(19)
C18 C16 P2 110.91(18)
C17 C16 H16 107.8
C18 C16 H16 107.8
P2 C16 H16 107.8
C16 C17 H17A 109.5
C16 C17 H17B 109.5
H17A C17 H17B 109.5
C16 C17 H17C 109.5
H17A C17 H17C 109.5
H17B C17 H17C 109.5
C16 C18 H18A 109.5
C16 C18 H18B 109.5
H18A C18 H18B 109.5
C16 C18 H18C 109.5
H18A C18 H18C 109.5
H18B C18 H18C 109.5
O2 N1 W1 178.97(18)
C11 N2 C10 110.45(18)
C11 N2 C2 109.93(18)
C10 N2 C2 108.37(18)
C11 N2 W1 116.67(15)
C10 N2 W1 118.08(14)
C2 N2 W1 91.18(13)
C2 O3 W1 99.96(15)
C9 P1 C6 105.76(12)
C9 P1 C3 104.28(12)
C6 P1 C3 104.64(12)
C9 P1 W1 102.61(8)
C6 P1 W1 119.21(8)
C3 P1 W1 118.63(9)
C16 P2 C12 104.22(12)
C16 P2 C13 108.00(12)
C12 P2 C13 100.20(12)
C16 P2 W1 118.98(9)
C12 P2 W1 102.57(8)
C13 P2 W1 119.60(9)
N1 W1 C1 88.61(10)
N1 W1 O3 172.47(8)
C1 W1 O3 98.47(9)
N1 W1 N2 112.15(8)
C1 W1 N2 159.24(9)
O3 W1 N2 60.83(7)
N1 W1 P2 94.55(6)
C1 W1 P2 100.76(7)
O3 W1 P2 81.65(5)
N2 W1 P2 78.82(5)
N1 W1 P1 94.37(6)
C1 W1 P1 99.96(7)
O3 W1 P1 86.99(5)
N2 W1 P1 78.79(5)
P2 W1 P1 157.60(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.159(3)
C1 W1 1.969(3)
C2 O4 1.208(3)
C2 O3 1.283(3)
C2 N2 1.512(3)
C3 C5 1.528(4)
C3 C4 1.530(4)
C3 P1 1.851(3)
C3 H3 0.9800
C4 H4A 0.9600
C4 H4B 0.9600
C4 H4C 0.9600
C5 H5A 0.9600
C5 H5B 0.9600
C5 H5C 0.9600
C6 C8 1.528(4)
C6 C7 1.530(4)
C6 P1 1.847(3)
C6 H6 0.9800
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C9 C10 1.526(4)
C9 P1 1.845(2)
C9 H9A 0.9700
C9 H9B 0.9700
C10 N2 1.498(3)
C10 H10A 0.9700
C10 H10B 0.9700
C11 N2 1.491(3)
C11 C12 1.526(3)
C11 H11A 0.9700
C11 H11B 0.9700
C12 P2 1.852(3)
C12 H12A 0.9700
C12 H12B 0.9700
C13 C15 1.521(4)
C13 C14 1.526(4)
C13 P2 1.852(3)
C13 H13 0.9800
C14 H14A 0.9600
C14 H14B 0.9600
C14 H14C 0.9600
C15 H15A 0.9600
C15 H15B 0.9600
C15 H15C 0.9600
C16 C17 1.528(4)
C16 C18 1.530(4)
C16 P2 1.844(3)
C16 H16 0.9800
C17 H17A 0.9600
C17 H17B 0.9600
C17 H17C 0.9600
C18 H18A 0.9600
C18 H18B 0.9600
C18 H18C 0.9600
N1 O2 1.208(3)
N1 W1 1.789(2)
N2 W1 2.2603(19)
O3 W1 2.2155(18)
P1 W1 2.4822(6)
P2 W1 2.4793(6)
