#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/83/1518348.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_1518348
loop_
_publ_author_name
'Graßl, C.'
'Bodensteiner, M.'
'Zabel, M.'
'Scheer, M.'
_publ_section_title
;
 Synthesis of arsenic-rich Asnligand complexes from yellow arsenic
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1379
_journal_paper_doi               10.1039/C4SC03543G
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C7 H7 Cr2 O7 P3'
_chemical_formula_sum            'C7 H7 Cr2 O7 P3'
_chemical_formula_weight         400.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-10-13 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                111.796(12)
_cell_angle_beta                 92.150(10)
_cell_angle_gamma                115.204(14)
_cell_formula_units_Z            1
_cell_length_a                   6.9134(9)
_cell_length_b                   7.3239(10)
_cell_length_c                   8.7610(10)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      66.4330
_cell_measurement_theta_min      5.5550
_cell_volume                     362.43(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega   29.60  116.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   37.0000  -30.0000 54

  2 omega   12.00  109.60   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000 -150.0000 61

  3 omega    8.00   89.60   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306 -125.0000  120.0000 51

  4 omega -121.00  -93.80   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  125.0000    0.0000 17

  5 omega   15.00  109.40   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -30.0000 59

  6 omega   29.00   73.80   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 28

  7 omega   94.00  126.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000  163.0000 20

  8 omega   63.00  160.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 61

  9 omega   19.00   65.40   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 29

 10 omega   40.00  161.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 76

 11 omega   17.00   68.20   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000  163.0000 32

 12 omega   10.00  131.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000   94.0000 76

 13 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000  150.0000 70

 14 omega  -37.00   63.80   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306  -37.0000  150.0000 63

 15 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000   60.0000 70

 16 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 70

 17 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -30.0000 70

 18 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 70

 19 omega   19.00   75.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 35

 20 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -60.0000 70

 21 omega   66.00  165.20   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 62

 22 omega  -97.00  -20.20   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6306  125.0000  -60.0000 48

 23 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000    0.0000 70

 24 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000  -60.0000 70

 25 omega   15.00   80.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -105.0000 41

 26 omega   60.00  117.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -150.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1375204000
_diffrn_orient_matrix_UB_12      0.1208994000
_diffrn_orient_matrix_UB_13      -0.0998276000
_diffrn_orient_matrix_UB_21      0.1121110000
_diffrn_orient_matrix_UB_22      0.2197174000
_diffrn_orient_matrix_UB_23      0.1626865000
_diffrn_orient_matrix_UB_31      0.1807011000
_diffrn_orient_matrix_UB_32      -0.0574347000
_diffrn_orient_matrix_UB_33      0.0385881000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4479
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.631
_diffrn_reflns_theta_min         5.592
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.728
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.014
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       plate
_exptl_crystal_F_000             198
_exptl_crystal_recrystallization_method
'The material was recrystallised from THF by cooling to -25'
_exptl_crystal_size_max          0.5603
_exptl_crystal_size_mid          0.1536
_exptl_crystal_size_min          0.0097
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0654P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1097
_reflns_number_total             1250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4sc03543g2.cif
_cod_data_source_block           neu
_cod_depositor_comments
'Adding full bibliography for 1518346--1518500.cif.'
_cod_original_cell_volume        362.42(9)
_cod_database_code               1518348
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C7 H7 O7 P3 W2'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 96.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All P(H,H) groups
 At 1.5 times of:
  All P(H,H,H) groups
2. Restrained distances
 P2-H2A = P2-H2B = P2-H2C = P3-H3A = P3-H3C = P3-H3B
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P2 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: P2(0.32) H2A(0.32) H2B(0.32) H2C(0.32) C4(0.82) O4(0.82) O2(0.68)
 C2(0.68) P3(0.18) H3A(0.18) H3B(0.18) H3C(0.18)
5.a Secondary CH2 refined with riding coordinates and stretchable bonds:
 P1(H1A,H1B)
5.b Idealised Me refined with riding coordinates and stretchable bonds:
 P2(H2A,H2B,H2C), P3(H3A,H3B,H3C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with inert oil'
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.08453(8) 0.66816(8) 0.67753(6) 0.0269(2) Uani 1 1 d . . . .
P1 P 0.03779(14) 0.30844(13) 0.55997(10) 0.0283(3) Uani 1 1 d . . . .
H1A H 0.218(4) 0.2926(3) 0.56467(13) 0.034 Uiso 1 1 calc GR . . .
H1B H -0.112(3) 0.168(3) 0.6042(9) 0.034 Uiso 1 1 calc GR . . .
P2 P 0.2222(19) 0.694(2) 0.9276(7) 0.0380(17) Uani 0.32 1 d D P A 1
H2A H 0.360(2) 0.613(2) 0.9070(7) 0.057 Uiso 0.32 1 calc DGR P A 1
H2B H 0.063(2) 0.580(2) 0.9821(8) 0.057 Uiso 0.32 1 calc DGR P A 1
H2C H 0.3234(19) 0.902(2) 1.0372(9) 0.057 Uiso 0.32 1 calc DGR P A 1
O1 O 0.5522(5) 0.8612(5) 0.6346(4) 0.0558(8) Uani 1 1 d . . . .
O3 O -0.3729(4) 0.4955(5) 0.7457(3) 0.0485(7) Uani 1 1 d . . . .
C4 C 0.121(3) 0.962(3) 0.800(2) 0.038(3) Uani 0.82 1 d . P A 2
O4 O 0.1406(7) 1.1354(7) 0.8731(5) 0.0504(10) Uani 0.82 1 d . P A 2
C1 C 0.3734(6) 0.7846(6) 0.6462(4) 0.0350(8) Uani 1 1 d . . . .
C3 C -0.2029(6) 0.5574(6) 0.7173(4) 0.0344(8) Uani 1 1 d . . . .
O2 O 0.2766(10) 0.6973(9) 1.0120(8) 0.0646(18) Uani 0.68 1 d . P A 2
C2 C 0.201(4) 0.683(4) 0.882(2) 0.0377(19) Uani 0.68 1 d . P A 2
P3 P 0.164(3) 1.020(3) 0.837(3) 0.036(3) Uani 0.18 1 d D P A 1
H3A H 0.199(3) 1.059(3) 0.996(3) 0.054 Uiso 0.18 1 calc DGR P A 1
H3B H 0.000(3) 1.052(3) 0.800(3) 0.054 Uiso 0.18 1 calc DGR P A 1
H3C H 0.340(3) 1.155(3) 0.809(3) 0.054 Uiso 0.18 1 calc DGR P A 1
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'
Cr Cr -0.1635 2.4439 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -4 3 0.0521 -0.0007 -4.0023 2.9989 -0.7834 -0.3916 0.3455
4 -2 1 0.2014 3.9944 -1.9936 1.0004 0.2084 0.1725 0.8749
-4 2 -1 0.3337 -3.9944 1.9936 -1.0004 -0.2084 -0.1725 -0.8749
-2 2 -1 0.2922 -1.9973 1.9975 -0.9999 0.0666 0.0523 -0.5142
0 0 1 0.0048 -0.0013 0.0005 1.0001 -0.0999 0.1627 0.0383
0 0 -1 0.0048 0.0013 -0.0005 -1.0001 0.0999 -0.1627 -0.0383
0 4 -3 0.0983 0.0007 4.0023 -2.9989 0.7834 0.3916 -0.3455
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
P1 Cr1 Cr1 50.30(3) . 2_566
P1 Cr1 Cr1 50.37(3) 2_566 2_566
P1 Cr1 P1 100.67(3) 2_566 .
P2 Cr1 Cr1 136.8(3) . 2_566
P2 Cr1 P1 86.5(3) . .
P2 Cr1 P1 172.6(3) . 2_566
C4 Cr1 Cr1 136.0(5) . 2_566
C4 Cr1 P1 85.7(5) . 2_566
C4 Cr1 P1 173.0(6) . .
C1 Cr1 Cr1 91.09(10) . 2_566
C1 Cr1 P1 89.82(11) . 2_566
C1 Cr1 P1 91.58(11) . .
C1 Cr1 P2 88.3(3) . .
C1 Cr1 C4 91.2(6) . .
C1 Cr1 C3 178.01(13) . .
C1 Cr1 P3 86.7(5) . .
C3 Cr1 Cr1 90.88(10) . 2_566
C3 Cr1 P1 91.63(10) . 2_566
C3 Cr1 P1 89.50(11) . .
C3 Cr1 P2 90.1(3) . .
C3 Cr1 C4 87.5(6) . .
C3 Cr1 P3 91.9(5) . .
C2 Cr1 Cr1 135.4(8) . 2_566
C2 Cr1 P1 85.1(8) . .
C2 Cr1 P1 173.8(8) . 2_566
C2 Cr1 C4 88.6(10) . .
C2 Cr1 C1 87.8(8) . .
C2 Cr1 C3 90.7(8) . .
P3 Cr1 Cr1 141.0(6) . 2_566
P3 Cr1 P1 168.6(6) . .
P3 Cr1 P1 90.7(6) . 2_566
P3 Cr1 P2 82.1(7) . .
Cr1 P1 Cr1 79.33(3) 2_566 .
Cr1 P1 H1A 115.4 . .
Cr1 P1 H1A 115.4 2_566 .
Cr1 P1 H1B 115.4 . .
Cr1 P1 H1B 115.4 2_566 .
H1A P1 H1B 112.4 . .
Cr1 P2 H2A 109.5 . .
Cr1 P2 H2B 109.5 . .
Cr1 P2 H2C 109.5 . .
H2A P2 H2B 109.5 . .
H2A P2 H2C 109.5 . .
H2B P2 H2C 109.5 . .
O4 C4 Cr1 179.4(17) . .
O1 C1 Cr1 177.0(3) . .
O3 C3 Cr1 178.1(3) . .
O2 C2 Cr1 179(2) . .
Cr1 P3 H3A 109.5 . .
Cr1 P3 H3B 109.5 . .
Cr1 P3 H3C 109.5 . .
H3A P3 H3B 109.5 . .
H3A P3 H3C 109.5 . .
H3B P3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 Cr1 2.9487(11) 2_566
Cr1 P1 2.3087(9) 2_566
Cr1 P1 2.3111(10) .
Cr1 P2 2.265(6) .
Cr1 C4 1.909(17) .
Cr1 C1 1.885(4) .
Cr1 C3 1.902(4) .
Cr1 C2 1.884(18) .
Cr1 P3 2.23(2) .
P1 Cr1 2.3087(9) 2_566
P1 H1A 1.30(3) .
P1 H1B 1.30(3) .
P2 H2A 1.299(6) .
P2 H2B 1.299(6) .
P2 H2C 1.299(6) .
O1 C1 1.147(5) .
O3 C3 1.141(5) .
C4 O4 1.134(17) .
O2 C2 1.182(15) .
P3 H3A 1.300(6) .
P3 H3B 1.300(6) .
P3 H3C 1.300(6) .
