#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025057.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_7025057
loop_
_publ_author_name
'Chmel, Nikola Paul'
'Howson, Suzanne E.'
'Allan, Laura E. N.'
'Barker, James'
'Clarkson, Guy J.'
'Turner, Scott S.'
'Scott, Peter'
_publ_section_title
;
 Organic-soluble optically pure anionic metal complexes
 PPh4[M(III)(S,S-EDDS)].2H2O (M = Fe, Co, Cr).
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2919
_journal_page_last               2927
_journal_paper_doi               10.1039/b924787d
_journal_volume                  39
_journal_year                    2010
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C34 H36 Co N2 O10 P'
_chemical_formula_weight         722.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            2
_cell_length_a                   16.9107(6)
_cell_length_b                   12.8825(4)
_cell_length_c                   7.3322(2)
_cell_measurement_reflns_used    25075
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.65
_cell_measurement_theta_min      2.76
_cell_volume                     1597.34(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'φ & ω 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            50153
_diffrn_reflns_theta_full        32.83
_diffrn_reflns_theta_max         32.83
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2459 Friedel pairs'
_refine_ls_abs_structure_Flack   0.009(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0303
_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)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                5017
_reflns_number_total             5741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924787d.txt
_cod_data_source_block           nc2
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               7025057
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-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
P1 P 0.0000 0.0000 0.93549(6) 0.02679(8) Uani 1 2 d S
C6 C 0.02934(7) 0.10390(10) 0.78963(19) 0.0306(2) Uani 1 1 d .
C7 C -0.02526(9) 0.14517(15) 0.6678(3) 0.0517(4) Uani 1 1 d .
H7A H -0.0771 0.1212 0.6681 0.062 Uiso 1 1 calc R
C8 C -0.00288(15) 0.22119(15) 0.5469(2) 0.0586(4) Uani 1 1 d .
H8A H -0.0399 0.2500 0.4681 0.070 Uiso 1 1 calc R
C9 C 0.07388(13) 0.25443(13) 0.5425(2) 0.0513(4) Uani 1 1 d .
H9A H 0.0890 0.3056 0.4601 0.062 Uiso 1 1 calc R
C10 C 0.12806(10) 0.21319(14) 0.6577(3) 0.0535(4) Uani 1 1 d .
H10A H 0.1804 0.2351 0.6515 0.064 Uiso 1 1 calc R
C11 C 0.10637(8) 0.13840(12) 0.7853(2) 0.0410(3) Uani 1 1 d .
H11A H 0.1435 0.1121 0.8667 0.049 Uiso 1 1 calc R
C12 C 0.07891(7) -0.03816(10) 1.08316(18) 0.0285(2) Uani 1 1 d .
C13 C 0.10672(10) -0.13851(12) 1.0881(3) 0.0462(4) Uani 1 1 d .
H13A H 0.0875 -0.1879 1.0070 0.055 Uiso 1 1 calc R
C14 C 0.16395(11) -0.16502(13) 1.2159(3) 0.0592(5) Uani 1 1 d .
H14A H 0.1831 -0.2326 1.2205 0.071 Uiso 1 1 calc R
C15 C 0.19233(8) -0.09219(15) 1.3352(2) 0.0476(4) Uani 1 1 d .
H15A H 0.2306 -0.1107 1.4203 0.057 Uiso 1 1 calc R
C16 C 0.16486(8) 0.00753(15) 1.3300(2) 0.0454(3) Uani 1 1 d .
H16A H 0.1848 0.0568 1.4106 0.055 Uiso 1 1 calc R
C17 C 0.10760(9) 0.03506(12) 1.2054(2) 0.0415(3) Uani 1 1 d .
H17A H 0.0882 0.1026 1.2032 0.050 Uiso 1 1 calc R
Co1 Co 0.0000 0.5000 0.14410(3) 0.02324(6) Uani 1 2 d S
O1 O 0.07132(5) 0.54168(8) 0.33311(12) 0.0349(2) Uani 1 1 d .
O2 O 0.18339(6) 0.59468(11) 0.45239(17) 0.0519(3) Uani 1 1 d .
O3 O 0.04179(5) 0.36291(7) 0.13821(14) 0.03288(19) Uani 1 1 d .
O4 O 0.15985(7) 0.28814(9) 0.11814(18) 0.0502(3) Uani 1 1 d .
N1 N 0.07674(6) 0.52392(8) -0.04283(14) 0.0273(2) Uani 1 1 d .
H1A H 0.0916 0.5833 -0.0489 0.033 Uiso 1 1 d R
C1 C 0.14613(7) 0.55514(11) 0.32727(18) 0.0326(3) Uani 1 1 d .
C2 C 0.19243(7) 0.52259(11) 0.1583(2) 0.0374(3) Uani 1 1 d .
H2A H 0.2140 0.5845 0.1017 0.045 Uiso 1 1 calc R
H2B H 0.2367 0.4801 0.1970 0.045 Uiso 1 1 calc R
C3 C 0.14628(7) 0.46308(11) 0.01569(18) 0.0324(3) Uani 1 1 d .
H3A H 0.1802 0.4487 -0.0896 0.039 Uiso 1 1 calc R
C4 C 0.11548(8) 0.36155(11) 0.09496(18) 0.0333(3) Uani 1 1 d .
C5 C 0.04331(8) 0.48672(12) -0.21890(17) 0.0359(3) Uani 1 1 d .
H5A H 0.0505 0.4123 -0.2304 0.043 Uiso 1 1 calc R
H5B H 0.0697 0.5204 -0.3204 0.043 Uiso 1 1 calc R
O5 O 0.31750(7) 0.19195(11) 0.2020(2) 0.0596(3) Uani 1 1 d .
H5D H 0.2751 0.2265 0.1872 0.089 Uiso 1 1 d R
H5C H 0.3095 0.1650 0.3071 0.089 Uiso 1 1 d 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
C6 P1 C6 106.32(9) 2 .
C6 P1 C12 111.38(6) 2 .
C6 P1 C12 111.22(6) . .
C6 P1 C12 111.22(6) 2 2
C6 P1 C12 111.38(6) . 2
C12 P1 C12 105.43(8) . 2
C11 C6 C7 119.35(13) . .
C11 C6 P1 121.28(11) . .
C7 C6 P1 119.17(10) . .
C8 C7 C6 120.27(16) . .
C8 C7 H7A 119.9 . .
C6 C7 H7A 119.9 . .
C9 C8 C7 119.99(17) . .
C9 C8 H8A 120.0 . .
C7 C8 H8A 120.0 . .
C10 C9 C8 120.31(15) . .
C10 C9 H9A 119.8 . .
C8 C9 H9A 119.8 . .
C9 C10 C11 120.81(15) . .
C9 C10 H10A 119.6 . .
C11 C10 H10A 119.6 . .
C6 C11 C10 119.21(15) . .
C6 C11 H11A 120.4 . .
C10 C11 H11A 120.4 . .
C13 C12 C17 120.12(13) . .
C13 C12 P1 121.97(10) . .
C17 C12 P1 117.71(10) . .
C12 C13 C14 119.11(15) . .
C12 C13 H13A 120.4 . .
C14 C13 H13A 120.4 . .
C15 C14 C13 120.42(15) . .
C15 C14 H14A 119.8 . .
C13 C14 H14A 119.8 . .
C16 C15 C14 120.48(14) . .
C16 C15 H15A 119.8 . .
C14 C15 H15A 119.8 . .
C15 C16 C17 119.96(15) . .
C15 C16 H16A 120.0 . .
C17 C16 H16A 120.0 . .
C16 C17 C12 119.91(14) . .
C16 C17 H17A 120.0 . .
C12 C17 H17A 120.0 . .
O3 Co1 O3 177.40(6) . 2_565
O3 Co1 N1 83.18(4) . .
O3 Co1 N1 94.95(4) 2_565 .
O3 Co1 N1 94.95(4) . 2_565
O3 Co1 N1 83.18(4) 2_565 2_565
N1 Co1 N1 88.44(6) . 2_565
O3 Co1 O1 92.45(4) . .
O3 Co1 O1 89.43(4) 2_565 .
N1 Co1 O1 92.65(4) . .
N1 Co1 O1 172.60(4) 2_565 .
O3 Co1 O1 89.43(4) . 2_565
O3 Co1 O1 92.45(4) 2_565 2_565
N1 Co1 O1 172.60(4) . 2_565
N1 Co1 O1 92.65(4) 2_565 2_565
O1 Co1 O1 87.21(5) . 2_565
C1 O1 Co1 129.62(9) . .
C4 O3 Co1 112.22(8) . .
C3 N1 C5 112.55(10) . .
C3 N1 Co1 104.27(7) . .
C5 N1 Co1 108.18(8) . .
C3 N1 H1A 105.8 . .
C5 N1 H1A 112.1 . .
Co1 N1 H1A 113.8 . .
O2 C1 O1 122.76(13) . .
O2 C1 C2 117.33(11) . .
O1 C1 C2 119.90(11) . .
C3 C2 C1 115.85(10) . .
C3 C2 H2A 108.3 . .
C1 C2 H2A 108.3 . .
C3 C2 H2B 108.3 . .
C1 C2 H2B 108.3 . .
H2A C2 H2B 107.4 . .
N1 C3 C2 110.04(11) . .
N1 C3 C4 107.12(10) . .
C2 C3 C4 110.34(11) . .
N1 C3 H3A 109.8 . .
C2 C3 H3A 109.8 . .
C4 C3 H3A 109.8 . .
O4 C4 O3 124.94(14) . .
O4 C4 C3 120.59(12) . .
O3 C4 C3 114.44(11) . .
N1 C5 C5 107.25(9) . 2_565
N1 C5 H5A 110.3 . .
C5 C5 H5A 110.3 2_565 .
N1 C5 H5B 110.3 . .
C5 C5 H5B 110.3 2_565 .
H5A C5 H5B 108.5 . .
H5D O5 H5C 101.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C6 1.7836(13) 2
P1 C6 1.7836(13) .
P1 C12 1.7874(13) .
P1 C12 1.7874(13) 2
C6 C11 1.3768(18) .
C6 C7 1.391(2) .
C7 C8 1.374(2) .
C7 H7A 0.9300 .
C8 C9 1.367(3) .
C8 H8A 0.9300 .
C9 C10 1.355(3) .
C9 H9A 0.9300 .
C10 C11 1.392(2) .
C10 H10A 0.9300 .
C11 H11A 0.9300 .
C12 C13 1.376(2) .
C12 C17 1.389(2) .
C13 C14 1.390(2) .
C13 H13A 0.9300 .
C14 C15 1.369(3) .
C14 H14A 0.9300 .
C15 C16 1.367(3) .
C15 H15A 0.9300 .
C16 C17 1.378(2) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
Co1 O3 1.9027(9) .
Co1 O3 1.9027(9) 2_565
Co1 N1 1.9125(10) .
Co1 N1 1.9125(10) 2_565
Co1 O1 1.9140(8) .
Co1 O1 1.9140(8) 2_565
O1 C1 1.2777(15) .
O2 C1 1.2240(16) .
O3 C4 1.2859(16) .
O4 C4 1.2191(17) .
N1 C3 1.4769(17) .
N1 C5 1.4886(17) .
N1 H1A 0.8062 .
C1 C2 1.5243(19) .
C2 C3 1.513(2) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.523(2) .
C3 H3A 0.9800 .
C5 C5 1.504(3) 2_565
C5 H5A 0.9700 .
C5 H5B 0.9700 .
O5 H5D 0.8509 .
O5 H5C 0.8560 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O5 0.81 2.36 3.0409(17) 142.2 4
O5 H5D O4 0.85 2.16 3.0035(16) 168.7 .
O5 H5C O2 0.86 1.99 2.8269(18) 167.2 4_546
C2 H2A O5 0.97 2.68 3.431(2) 135.0 4
C13 H13A O5 0.93 2.71 3.307(2) 123.1 4_546
C5 H5B O1 0.97 2.56 3.3934(15) 144.6 1_554
C5 H5B O2 0.97 2.72 3.6545(19) 162.4 1_554
