#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:01:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179713 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/15/7001588.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_7001588
loop_
_publ_author_name
'Edwards, Peter G.'
'Hahn, F. Ekkehardt'
'Limon, Matthieu'
'Newman, Paul D.'
'Kariuki, Benson M.'
'Stasch, Andreas'
_publ_section_title
;
 Manganese complexes of phosphino-μ-phosphido ligands
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5115
_journal_page_last               5119
_journal_paper_doi               10.1039/b822870a
_journal_year                    2009
_chemical_formula_moiety         'C18 H14 Mn2 O6 P4, C4 H8 O'
_chemical_formula_sum            'C22 H22 Mn2 O7 P4'
_chemical_formula_weight         632.16
_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                 94.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3011(19)
_cell_length_b                   19.035(4)
_cell_length_c                   14.797(3)
_cell_measurement_reflns_used    257
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      3.50
_cell_volume                     2609.8(9)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD 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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5598
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0251
_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)+(0.0248P)²+2.5062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                2574
_reflns_number_total             2842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822870a.txt
_cod_data_source_block           ASPGE01
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7001588
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
Mn1 Mn 0.07852(2) 0.267328(12) 0.051716(16) 0.02252(8) Uani 1 1 d . . .
P1 P 0.24850(4) 0.17938(2) 0.03279(3) 0.02248(10) Uani 1 1 d . . .
O1 O -0.10868(16) 0.18012(7) 0.15823(10) 0.0462(4) Uani 1 1 d . . .
C1 C 0.15400(17) 0.10822(8) -0.03029(11) 0.0239(3) Uani 1 1 d . . .
H1 H 0.3021(19) 0.1448(10) 0.1053(12) 0.030(5) Uiso 1 1 d . . .
P2 P -0.02880(5) 0.21738(2) -0.07626(3) 0.02655(11) Uani 1 1 d . . .
O2 O -0.10824(16) 0.39346(7) 0.04138(11) 0.0494(4) Uani 1 1 d . . .
C2 C 0.02718(18) 0.12598(8) -0.08369(11) 0.0251(3) Uani 1 1 d . . .
O3 O 0.22898(16) 0.31556(8) 0.22495(9) 0.0449(3) Uani 1 1 d . . .
C3 C -0.04847(19) 0.07532(9) -0.13649(11) 0.0296(4) Uani 1 1 d . . .
H3 H -0.1334 0.0876 -0.1734 0.036 Uiso 1 1 calc R . .
O4 O 0.5000 -0.12439(11) -0.2500 0.0509(5) Uani 1 2 d S . .
C4 C 0.0018(2) 0.00653(9) -0.13460(12) 0.0325(4) Uani 1 1 d . . .
H4 H -0.0503 -0.0286 -0.1694 0.039 Uiso 1 1 calc R . .
C5 C 0.1270(2) -0.01113(9) -0.08248(12) 0.0312(4) Uani 1 1 d . . .
H5 H 0.1606 -0.0583 -0.0819 0.037 Uiso 1 1 calc R . .
C6 C 0.20434(19) 0.03938(8) -0.03092(12) 0.0279(3) Uani 1 1 d . . .
H6 H 0.2914 0.0270 0.0038 0.034 Uiso 1 1 calc R . .
C7 C -0.0365(2) 0.21366(9) 0.11602(12) 0.0303(4) Uani 1 1 d . . .
C8 C -0.03733(19) 0.34405(9) 0.04443(12) 0.0314(4) Uani 1 1 d . . .
C9 C 0.17388(19) 0.29707(9) 0.15678(12) 0.0294(4) Uani 1 1 d . . .
C10 C 0.6025(2) -0.08093(13) -0.28888(15) 0.0513(5) Uani 1 1 d . . .
H10A H 0.5885 -0.0830 -0.3559 0.062 Uiso 1 1 calc R . .
H10B H 0.7018 -0.0966 -0.2693 0.062 Uiso 1 1 calc R . .
C11 C 0.5788(3) -0.00769(15) -0.2566(2) 0.0707(8) Uani 1 1 d . . .
H11A H 0.6377 0.0020 -0.1989 0.085 Uiso 1 1 calc R . .
H11B H 0.6019 0.0274 -0.3025 0.085 Uiso 1 1 calc R . .
H2A H -0.172(2) 0.2134(11) -0.0824(14) 0.040(6) Uiso 1 1 d . . .
H2B H -0.008(2) 0.2431(11) -0.1594(14) 0.043(6) Uiso 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'
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'
Mn Mn 0.3368 0.7283 '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
C7 Mn1 C9 89.59(8) . . ?
C7 Mn1 C8 96.35(8) . . ?
C9 Mn1 C8 92.49(8) . . ?
C7 Mn1 P2 87.99(6) . . ?
C9 Mn1 P2 173.18(6) . . ?
C8 Mn1 P2 94.12(6) . . ?
C7 Mn1 P1 95.50(6) . . ?
C9 Mn1 P1 92.34(6) . . ?
C8 Mn1 P1 167.23(6) . . ?
P2 Mn1 P1 81.55(3) . . ?
C7 Mn1 P1 170.66(6) . 7 ?
C9 Mn1 P1 90.86(6) . 7 ?
C8 Mn1 P1 92.95(6) . 7 ?
P2 Mn1 P1 90.49(2) . 7 ?
P1 Mn1 P1 75.16(2) . 7 ?
C1 P1 Mn1 106.98(6) . . ?
C1 P1 Mn1 111.67(5) . 7 ?
Mn1 P1 Mn1 104.84(2) . 7 ?
C6 C1 C2 119.34(15) . . ?
C6 C1 P1 123.67(13) . . ?
C2 C1 P1 116.93(12) . . ?
C2 P2 Mn1 110.05(6) . . ?
C3 C2 C1 120.55(15) . . ?
C3 C2 P2 124.18(13) . . ?
C1 C2 P2 115.26(12) . . ?
C4 C3 C2 119.23(16) . . ?
C10 O4 C10 108.8(2) 2_654 . ?
C5 C4 C3 120.43(16) . . ?
C4 C5 C6 120.62(16) . . ?
C5 C6 C1 119.81(17) . . ?
O1 C7 Mn1 178.82(16) . . ?
O2 C8 Mn1 178.26(17) . . ?
O3 C9 Mn1 177.15(16) . . ?
O4 C10 C11 106.88(18) . . ?
C11 C11 C10 102.41(16) 2_654 . ?
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
Mn1 C7 1.8084(19) . ?
Mn1 C9 1.8123(19) . ?
Mn1 C8 1.8125(18) . ?
Mn1 P2 2.2710(7) . ?
Mn1 P1 2.3361(6) . ?
Mn1 P1 2.3518(7) 7 ?
P1 C1 1.8264(17) . ?
P1 Mn1 2.3518(7) 7 ?
O1 C7 1.150(2) . ?
C1 C6 1.392(2) . ?
C1 C2 1.403(2) . ?
P2 C2 1.8221(17) . ?
O2 C8 1.147(2) . ?
C2 C3 1.393(2) . ?
O3 C9 1.146(2) . ?
C3 C4 1.390(3) . ?
O4 C10 1.421(2) 2_654 ?
O4 C10 1.421(2) . ?
C4 C5 1.382(3) . ?
C5 C6 1.389(2) . ?
C10 C11 1.496(3) . ?
C11 C11 1.495(5) 2_654 ?
