#------------------------------------------------------------------------------
#$Date: 2017-09-21 05:22:53 +0300 (Thu, 21 Sep 2017) $
#$Revision: 201096 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044295.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_7044295
loop_
_publ_author_name
'Feng, Yutian'
'Phelps, Tim E.'
'Carroll, Valerie'
'Gallazzi, Fabio'
'Sieckman, Gary'
'Hoffman, Timothy J.'
'Barnes, Charles L.'
'Ketring, Alan R.'
'Hennkens, Heather M.'
'Jurisson, Silvia'
_publ_section_title
;
 Chemistry and Radiochemistry of Arsenic, Rhenium and Rhodium Isotopes
 Relevant to Radiopharmaceutical Applications: Development of High
 Specific Activity Radionuclides for Imaging and Treatment
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02407J
_journal_year                    2017
_chemical_formula_moiety         'C6 H11 As O3'
_chemical_formula_sum            'C6 H11 As O3'
_chemical_formula_weight         206.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-01 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.0059(10)
_cell_length_b                   11.602(2)
_cell_length_c                   10.6270(18)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     739.9(2)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8432
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         2.600
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    4.537
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       Rod
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0314P)²+0.4585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1568
_reflns_number_total             1691
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02407j2.cif
_cod_data_source_block           20141026Feng
_cod_database_code               7044295
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.210
_shelx_estimated_absorpt_t_max   0.549
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
As1 As 0.77408(3) 0.44052(2) 0.60634(2) 0.01457(8) Uani 1 1 d . .
O1 O 0.7335(2) 0.31889(11) 0.50631(12) 0.0154(3) Uani 1 1 d . .
O2 O 0.7471(2) 0.36462(12) 0.75101(12) 0.0182(3) Uani 1 1 d . .
O3 O 1.0716(2) 0.44101(10) 0.61051(14) 0.0169(3) Uani 1 1 d . .
C1 C 0.8995(3) 0.22888(16) 0.52295(17) 0.0140(3) Uani 1 1 d . .
H1A H 1.0111 0.2369 0.4574 0.017 Uiso 1 1 calc R U
H1B H 0.8266 0.1529 0.5117 0.017 Uiso 1 1 calc R U
C2 C 0.8446(3) 0.25021(17) 0.75399(17) 0.0164(4) Uani 1 1 d . .
H2A H 0.7247 0.1924 0.7408 0.020 Uiso 1 1 calc R U
H2B H 0.9160 0.2365 0.8382 0.020 Uiso 1 1 calc R U
C3 C 1.1773(3) 0.33703(15) 0.65839(18) 0.0155(4) Uani 1 1 d . .
H3A H 1.2305 0.3499 0.7466 0.019 Uiso 1 1 calc R U
H3B H 1.3085 0.3196 0.6082 0.019 Uiso 1 1 calc R U
C4 C 1.0186(3) 0.23355(15) 0.65335(16) 0.0126(3) Uani 1 1 d . .
C5 C 1.1452(3) 0.12093(16) 0.68165(18) 0.0163(4) Uani 1 1 d . .
H5A H 1.2279 0.1293 0.7636 0.020 Uiso 1 1 calc R U
H5B H 1.0350 0.0583 0.6908 0.020 Uiso 1 1 calc R U
C6 C 1.3100(3) 0.08424(17) 0.58281(19) 0.0178(4) Uani 1 1 d . .
H6A H 1.2291 0.0698 0.5025 0.027 Uiso 1 1 calc R U
H6B H 1.3869 0.0137 0.6108 0.027 Uiso 1 1 calc R U
H6C H 1.4195 0.1457 0.5719 0.027 Uiso 1 1 calc R U
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'
As As 0.0499 2.0058 '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 As1 O2 96.23(6)
O1 As1 O3 97.51(6)
O2 As1 O3 96.03(6)
C1 O1 As1 114.93(10)
C2 O2 As1 114.84(11)
C3 O3 As1 115.51(11)
O1 C1 C4 112.22(14)
O1 C1 H1A 109.2
C4 C1 H1A 109.2
O1 C1 H1B 109.2
C4 C1 H1B 109.2
H1A C1 H1B 107.9
O2 C2 C4 112.63(15)
O2 C2 H2A 109.1
C4 C2 H2A 109.1
O2 C2 H2B 109.1
C4 C2 H2B 109.1
H2A C2 H2B 107.8
O3 C3 C4 112.19(14)
O3 C3 H3A 109.2
C4 C3 H3A 109.2
O3 C3 H3B 109.2
C4 C3 H3B 109.2
H3A C3 H3B 107.9
C3 C4 C1 109.02(14)
C3 C4 C5 110.93(15)
C1 C4 C5 110.87(15)
C3 C4 C2 108.43(15)
C1 C4 C2 109.12(15)
C5 C4 C2 108.42(15)
C6 C5 C4 115.51(15)
C6 C5 H5A 108.4
C4 C5 H5A 108.4
C6 C5 H5B 108.4
C4 C5 H5B 108.4
H5A C5 H5B 107.5
C5 C6 H6A 109.5
C5 C6 H6B 109.5
H6A C6 H6B 109.5
C5 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
As1 O1 1.7777(13)
As1 O2 1.7847(14)
As1 O3 1.7858(14)
O1 C1 1.450(2)
O2 C2 1.451(2)
O3 C3 1.446(2)
C1 C4 1.535(2)
C1 H1A 0.9900
C1 H1B 0.9900
C2 C4 1.537(2)
C2 H2A 0.9900
C2 H2B 0.9900
C3 C4 1.533(2)
C3 H3A 0.9900
C3 H3B 0.9900
C4 C5 1.536(2)
C5 C6 1.532(3)
C5 H5A 0.9900
C5 H5B 0.9900
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O2 As1 O1 C1 -62.17(12)
O3 As1 O1 C1 34.77(12)
O1 As1 O2 C2 37.75(13)
O3 As1 O2 C2 -60.52(13)
O1 As1 O3 C3 -59.04(13)
O2 As1 O3 C3 38.08(13)
As1 O1 C1 C4 22.57(18)
As1 O2 C2 C4 20.13(19)
As1 O3 C3 C4 19.77(19)
O3 C3 C4 C1 47.3(2)
O3 C3 C4 C5 169.67(15)
O3 C3 C4 C2 -71.38(18)
O1 C1 C4 C3 -72.75(18)
O1 C1 C4 C5 164.85(14)
O1 C1 C4 C2 45.51(19)
O2 C2 C4 C3 47.81(19)
O2 C2 C4 C1 -70.81(19)
O2 C2 C4 C5 168.33(15)
C3 C4 C5 C6 -67.0(2)
C1 C4 C5 C6 54.3(2)
C2 C4 C5 C6 174.09(16)
