#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179338 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/35/4323523.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_4323523
loop_
_publ_author_name
'Donald J. Darensbourg'
'Jennifer D. Draper'
'Joseph H. Reibenspies'
_publ_section_title
;
 Amino Acid Complexes of Metal Carbonyls: Mechanistic Aspects of the
 CO-Labilizing Ability of Glycinate Ligands in Zero-Valent Chromium and
 Tungsten Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3648
_journal_page_last               3656
_journal_paper_doi               10.1021/ic961344m
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C15 H22 N2 O6 P W'
_chemical_formula_weight         541.17
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.101(2)
_cell_length_b                   13.310(2)
_cell_length_c                   14.130(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3203.4(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4980
_diffrn_reflns_theta_max         60.12
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    7.331
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_F_000             1052
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.157
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_obs          0.0324
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0798
_refine_ls_wR_factor_obs         0.0753
_reflns_number_observed          3925
_reflns_number_total             4754
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961344m_5.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323523
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.744902(13) 0.48983(2) 0.14982(2) 0.04391(10) Uani 1 d . .
P1 P 0.68816(7) 0.56314(9) 0.29171(9) 0.0409(3) Uani 1 d . .
O3 O 0.8466(3) 0.4030(4) -0.0048(3) 0.091(2) Uani 1 d . .
O1 O 0.7301(3) 0.6986(4) 0.0432(3) 0.093(2) Uani 1 d . .
O2 O 0.7313(3) 0.2700(3) 0.2304(4) 0.0812(14) Uani 1 d . .
O4 O 0.5921(3) 0.4356(4) 0.0237(3) 0.0850(14) Uani 1 d . .
O5 O 0.9097(2) 0.6167(3) 0.3689(3) 0.0545(9) Uani 1 d . .
O6 O 0.8487(2) 0.5345(3) 0.2484(3) 0.0485(8) Uani 1 d . .
O7 O 0.7461(3) 0.8858(4) 0.2393(4) 0.101(2) Uani 1 d . .
N1 N 0.9775(3) 0.6732(3) 0.6868(3) 0.0560(12) Uani 1 d . .
C3 C 0.8095(3) 0.4364(5) 0.0527(4) 0.0592(15) Uani 1 d . .
C1 C 0.7372(3) 0.6245(5) 0.0853(4) 0.0578(15) Uani 1 d . .
C2 C 0.7389(3) 0.3501(4) 0.2045(4) 0.0527(14) Uani 1 d . .
C4 C 0.6492(3) 0.4556(4) 0.0698(4) 0.0556(14) Uani 1 d . .
C5 C 0.7713(3) 0.6392(4) 0.3414(4) 0.0461(13) Uani 1 d . .
H5A H 0.7670(3) 0.7064(4) 0.3148(4) 0.055 Uiso 1 calc R .
H5B H 0.7696(3) 0.6447(4) 0.4097(4) 0.055 Uiso 1 calc R .
C6 C 0.8490(3) 0.5932(3) 0.3201(4) 0.0414(12) Uani 1 d . .
C7 C 0.6690(3) 0.4761(4) 0.3858(4) 0.0443(12) Uani 1 d . .
C8 C 0.7288(4) 0.4173(4) 0.4272(4) 0.064(2) Uani 1 d . .
H8A H 0.7796(4) 0.4269(4) 0.4101(4) 0.077 Uiso 1 calc R .
C9 C 0.7155(4) 0.3447(5) 0.4934(5) 0.079(2) Uani 1 d . .
H9A H 0.7570(4) 0.3064(5) 0.5209(5) 0.095 Uiso 1 calc R .
C10 C 0.6414(5) 0.3292(5) 0.5183(5) 0.076(2) Uani 1 d . .
H10A H 0.6323(5) 0.2794(5) 0.5622(5) 0.091 Uiso 1 calc R .
C11 C 0.5809(4) 0.3856(5) 0.4799(5) 0.071(2) Uani 1 d . .
H11A H 0.5306(4) 0.3749(5) 0.4980(5) 0.085 Uiso 1 calc R .
C12 C 0.5939(3) 0.4599(4) 0.4131(4) 0.0580(14) Uani 1 d . .
H12A H 0.5522(3) 0.4986(4) 0.3869(4) 0.070 Uiso 1 calc R .
C13 C 0.6045(3) 0.6471(4) 0.2855(4) 0.0481(13) Uani 1 d . .
C14 C 0.5936(3) 0.7124(4) 0.3593(5) 0.063(2) Uani 1 d . .
H14A H 0.6294(3) 0.7131(4) 0.4129(5) 0.076 Uiso 1 calc R .
C15 C 0.5294(4) 0.7770(5) 0.3540(6) 0.077(2) Uani 1 d . .
H15A H 0.5223(4) 0.8212(5) 0.4034(6) 0.093 Uiso 1 calc R .
C16 C 0.4762(4) 0.7746(5) 0.2744(7) 0.091(3) Uani 1 d . .
H16A H 0.4333(4) 0.8177(5) 0.2702(7) 0.110 Uiso 1 calc R .
C17 C 0.4863(4) 0.7101(6) 0.2026(6) 0.085(2) Uani 1 d . .
H17A H 0.4497(4) 0.7087(6) 0.1499(6) 0.102 Uiso 1 calc R .
C18 C 0.5506(3) 0.6458(5) 0.2064(5) 0.063(2) Uani 1 d . .
H18A H 0.5573(3) 0.6024(5) 0.1563(5) 0.076 Uiso 1 calc R .
C19 C 1.0633(3) 0.7038(5) 0.7076(5) 0.078(2) Uani 1 d . .
H19A H 1.0935(3) 0.6446(5) 0.7275(5) 0.094 Uiso 1 calc R .
H19B H 1.0826(3) 0.7277(5) 0.6491(5) 0.094 Uiso 1 calc R .
C20 C 1.0786(4) 0.7845(5) 0.7832(7) 0.121(4) Uani 1 d . .
H20A H 1.1338(4) 0.7990(5) 0.7915(7) 0.182 Uiso 1 calc R .
H20B H 1.0614(4) 0.7612(5) 0.8421(7) 0.182 Uiso 1 calc R .
H20C H 1.0504(4) 0.8444(5) 0.7636(7) 0.182 Uiso 1 calc R .
C21 C 0.9426(3) 0.6435(4) 0.7774(4) 0.0582(15) Uani 1 d . .
H21A H 0.9445(3) 0.7012(4) 0.8194(4) 0.070 Uiso 1 calc R .
H21B H 0.8878(3) 0.6266(4) 0.7619(4) 0.070 Uiso 1 calc R .
C22 C 0.9821(4) 0.5567(5) 0.8302(5) 0.080(2) Uani 1 d . .
H22A H 0.9562(4) 0.5432(5) 0.8864(5) 0.120 Uiso 1 calc R .
H22B H 1.0361(4) 0.5731(5) 0.8478(5) 0.120 Uiso 1 calc R .
H22C H 0.9793(4) 0.4982(5) 0.7902(5) 0.120 Uiso 1 calc R .
C23 C 0.9759(4) 0.5858(4) 0.6170(5) 0.068(2) Uani 1 d . .
H23A H 0.9965(4) 0.6089(4) 0.5590(5) 0.081 Uiso 1 calc R .
H23B H 1.0107(4) 0.5336(4) 0.6439(5) 0.081 Uiso 1 calc R .
C24 C 0.8966(4) 0.5406(5) 0.5918(5) 0.081(2) Uani 1 d . .
H24A H 0.9010(4) 0.4864(5) 0.5478(5) 0.121 Uiso 1 calc R .
H24B H 0.8618(4) 0.5910(5) 0.5633(5) 0.121 Uiso 1 calc R .
H24C H 0.8760(4) 0.5156(5) 0.6483(5) 0.121 Uiso 1 calc R .
C25 C 0.9282(3) 0.7603(4) 0.6460(4) 0.063(2) Uani 1 d . .
H25A H 0.8737(3) 0.7390(4) 0.6387(4) 0.076 Uiso 1 calc R .
H25B H 0.9321(3) 0.8147(4) 0.6919(4) 0.076 Uiso 1 calc R .
C26 C 0.9491(4) 0.8010(5) 0.5520(5) 0.084(2) Uani 1 d . .
H26A H 0.9145(4) 0.8555(5) 0.5328(5) 0.126 Uiso 1 calc R .
H26B H 0.9437(4) 0.7487(5) 0.5051(5) 0.126 Uiso 1 calc R .
H26C H 1.0023(4) 0.8246(5) 0.5584(5) 0.126 Uiso 1 calc R .
C27 C 0.7430(6) 0.9445(9) 0.3187(7) 0.134(4) Uani 1 d . .
H27A H 0.7914(6) 0.9824(9) 0.3297(7) 0.161 Uiso 1 calc R .
H27B H 0.7381(6) 0.9019(9) 0.3735(7) 0.161 Uiso 1 calc R .
C28 C 0.6796(8) 1.0110(8) 0.3086(9) 0.164(5) Uani 1 d . .
H28A H 0.6983(8) 1.0798(8) 0.3075(9) 0.196 Uiso 1 calc R .
H28B H 0.6474(8) 1.0036(8) 0.3613(9) 0.196 Uiso 1 calc R .
C29 C 0.6348(6) 0.9874(8) 0.2208(8) 0.134(4) Uani 1 d . .
H29A H 0.6288(6) 1.0462(8) 0.1804(8) 0.161 Uiso 1 calc R .
H29B H 0.5830(6) 0.9629(8) 0.2325(8) 0.161 Uiso 1 calc R .
C30 C 0.6797(6) 0.9086(7) 0.1760(6) 0.108(3) Uani 1 d . .
H30A H 0.6475(6) 0.8492(7) 0.1641(6) 0.130 Uiso 1 calc R .
H30B H 0.6960(6) 0.9324(7) 0.1160(6) 0.130 Uiso 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 0.0181 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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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
C4 W1 C3 90.3(2) . . ?
C4 W1 C1 85.8(2) . . ?
C3 W1 C1 91.4(2) . . ?
C4 W1 C2 86.5(2) . . ?
C3 W1 C2 89.1(2) . . ?
C1 W1 C2 172.3(2) . . ?
C4 W1 O6 175.8(2) . . ?
C3 W1 O6 93.8(2) . . ?
C1 W1 O6 93.6(2) . . ?
C2 W1 O6 94.1(2) . . ?
C4 W1 P1 100.9(2) . . ?
C3 W1 P1 168.7(2) . . ?
C1 W1 P1 90.1(2) . . ?
C2 W1 P1 90.9(2) . . ?
O6 W1 P1 74.97(9) . . ?
C13 P1 C7 103.7(2) . . ?
C13 P1 C5 105.1(2) . . ?
C7 P1 C5 104.9(2) . . ?
C13 P1 W1 124.2(2) . . ?
C7 P1 W1 116.5(2) . . ?
C5 P1 W1 100.3(2) . . ?
C6 O6 W1 127.0(3) . . ?
C27 O7 C30 107.9(6) . . ?
C21 N1 C25 105.8(4) . . ?
C21 N1 C23 111.2(4) . . ?
C25 N1 C23 111.1(5) . . ?
C21 N1 C19 110.6(5) . . ?
C25 N1 C19 111.3(4) . . ?
C23 N1 C19 106.9(4) . . ?
O3 C3 W1 178.5(6) . . ?
O1 C1 W1 175.5(5) . . ?
O2 C2 W1 175.1(5) . . ?
O4 C4 W1 179.0(5) . . ?
C6 C5 P1 111.3(3) . . ?
O5 C6 O6 122.8(4) . . ?
O5 C6 C5 119.6(5) . . ?
O6 C6 C5 117.6(4) . . ?
C8 C7 C12 117.7(5) . . ?
C8 C7 P1 119.9(4) . . ?
C12 C7 P1 122.3(4) . . ?
C7 C8 C9 121.7(6) . . ?
C10 C9 C8 119.7(6) . . ?
C11 C10 C9 120.6(6) . . ?
C10 C11 C12 120.1(6) . . ?
C7 C12 C11 120.2(6) . . ?
C18 C13 C14 119.4(5) . . ?
C18 C13 P1 119.9(4) . . ?
C14 C13 P1 120.7(4) . . ?
C13 C14 C15 120.4(6) . . ?
C16 C15 C14 119.3(7) . . ?
C17 C16 C15 120.4(7) . . ?
C16 C17 C18 121.0(7) . . ?
C13 C18 C17 119.4(7) . . ?
C20 C19 N1 115.2(5) . . ?
C22 C21 N1 115.3(5) . . ?
C24 C23 N1 115.1(5) . . ?
C26 C25 N1 116.2(5) . . ?
O7 C27 C28 111.3(9) . . ?
C27 C28 C29 107.5(9) . . ?
C28 C29 C30 105.6(9) . . ?
O7 C30 C29 107.5(7) . . ?
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 C4 1.959(6) . ?
W1 C3 1.970(6) . ?
W1 C1 2.010(6) . ?
W1 C2 2.020(6) . ?
W1 O6 2.237(3) . ?
W1 P1 2.5021(13) . ?
P1 C13 1.811(5) . ?
P1 C7 1.816(5) . ?
P1 C5 1.834(5) . ?
O3 C3 1.162(7) . ?
O1 C1 1.153(7) . ?
O2 C2 1.139(6) . ?
O4 C4 1.155(7) . ?
O5 C6 1.234(6) . ?
O6 C6 1.279(6) . ?
O7 C27 1.372(9) . ?
O7 C30 1.414(9) . ?
N1 C21 1.513(7) . ?
N1 C25 1.517(6) . ?
N1 C23 1.524(7) . ?
N1 C19 1.526(7) . ?
C5 C6 1.518(6) . ?
C7 C8 1.376(7) . ?
C7 C12 1.391(7) . ?
C8 C9 1.378(8) . ?
C9 C10 1.361(9) . ?
C10 C11 1.353(9) . ?
C11 C12 1.399(8) . ?
C13 C18 1.383(8) . ?
C13 C14 1.384(8) . ?
C14 C15 1.391(8) . ?
C15 C16 1.381(10) . ?
C16 C17 1.352(11) . ?
C17 C18 1.390(8) . ?
C19 C20 1.521(9) . ?
C21 C22 1.503(8) . ?
C23 C24 1.497(9) . ?
C25 C26 1.506(8) . ?
C27 C28 1.396(13) . ?
C28 C29 1.433(14) . ?
C29 C30 1.475(11) . ?
