Synthesis of arsenic-rich Asnligand complexes from yellow arsenic
Graßl, C.; Bodensteiner, M.; Zabel, M.; Scheer, M.; Chem. Sci. 6 (2015) 1379–; doi:10.1039/C4SC03543G

data_1518496
_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         'C34 H58 As4 Co2'
_chemical_formula_sum            'C34 H58 As4 Co2'
_chemical_formula_weight         884.34
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-10 deposited with the CCDC.
2014-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.43860(10)
_cell_length_b                   13.76760(10)
_cell_length_c                   16.02760(10)
_cell_measurement_reflns_used    14595
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      66.5503
_cell_measurement_theta_min      2.7917
_cell_volume                     1832.24(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
(compiled Jun 18 2008,17:52:12)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
(compiled Jun 18 2008,17:52:12)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
(compiled Jun 18 2008,17:52:12)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.0(2)
_diffrn_detector_area_resol_mean 10.5431
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;
  1 omega  -14.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
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  2 omega  -86.00  -33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  150.0000    0.0000    0.0000 53

  3 omega  -37.00   16.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  180.0000    0.0000    0.0000 53

  4 omega   33.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000  120.0000    0.0000    0.0000 53

  5 omega   10.00   63.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000  300.0000    0.0000    0.0000 53

  6 omega  -37.00   16.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  330.0000    0.0000    0.0000 53

  7 omega -115.00  -61.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  109.0000  274.0000    0.0000    0.0000 54

  8 omega -118.00  -65.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   45.0000  150.0000    0.0000    0.0000 53

  9 omega -178.00  -87.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  150.0000    0.0000    0.0000 91

 10 omega -111.00  -57.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  100.0000  181.0000    0.0000    0.0000 54

 11 omega -124.00  -65.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
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 12 omega -124.00  -22.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
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 13 omega -118.00  -64.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   45.0000    0.0000    0.0000    0.0000 54

 14 omega -117.00  -63.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  115.0000   42.0000    0.0000    0.0000 54

 15 omega   69.00  127.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  180.0000    0.0000    0.0000 58

 16 omega    4.00   64.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000  150.0000    0.0000    0.0000 60

 17 omega   66.00  119.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   30.0000    0.0000    0.0000 53

 18 omega   66.00  119.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000    0.0000    0.0000    0.0000 53

 19 omega   66.00  119.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  270.0000    0.0000    0.0000 53

 20 omega   68.00  121.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  300.0000    0.0000    0.0000 53

 21 omega   68.00  121.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000   60.0000    0.0000    0.0000 53

 22 omega   66.00  119.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  120.0000    0.0000    0.0000 53

 23 omega   69.00  127.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000   60.0000    0.0000    0.0000 58

 24 omega  115.00  168.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 53

 25 omega   69.00  127.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  270.0000    0.0000    0.0000 58

 26 omega   68.00  121.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  180.0000    0.0000    0.0000 53

 27 omega  114.00  172.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000   90.0000    0.0000    0.0000 58

 28 omega -178.00   -1.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  300.0000    0.0000    0.0000 177

 29 omega -178.00  -35.00   1.0000    7.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  120.0000    0.0000    0.0000 143
;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_orient_matrix_UB_11      0.1416408943
_diffrn_orient_matrix_UB_12      0.0486180910
_diffrn_orient_matrix_UB_13      -0.0326116319
_diffrn_orient_matrix_UB_21      0.0477434121
_diffrn_orient_matrix_UB_22      -0.0988439663
_diffrn_orient_matrix_UB_23      -0.0331241115
_diffrn_orient_matrix_UB_31      -0.1097538450
_diffrn_orient_matrix_UB_32      0.0197128366
_diffrn_orient_matrix_UB_33      -0.0858978425
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19971
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.683
_diffrn_reflns_theta_min         4.263
_diffrn_source                   'Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
(compiled Jun 18 2008,17:52:12)
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    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_recrystallization_method
'The material was recrystallised from a saturated hexane solution at -25 degree celsius.'
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3018
_reflns_number_total             3181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03543g1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1518346--1518500.cif.'
_cod_database_code               1518496
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.185
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.019) H5(0.019) H7A(0.049) H7B(0.049) H7C(0.049) H8A(0.047)
 H8B(0.047) H8C(0.047) H9A(0.04) H9B(0.04) H9C(0.04) H11A(0.031) H11B(0.031)
 H11C(0.031) H12A(0.035) H12B(0.035) H12C(0.035) H13A(0.031) H13B(0.031)
 H13C(0.031) H15A(0.038) H15B(0.038) H15C(0.038) H16A(0.042) H16B(0.042)
 H16C(0.042) H17A(0.043) H17B(0.043) H17C(0.043)
 Fixed X: H2(0.8755) H5(0.433999) H7A(0.766399) H7B(0.8762) H7C(0.9249)
 H8A(0.930499) H8B(0.8846) H8C(0.778) H9A(0.527) H9B(0.638) H9C(0.5308)
 H11A(0.8598) H11B(0.9649) H11C(0.981999) H12A(0.9192) H12B(0.7667)
 H12C(0.916399) H13A(0.622901) H13B(0.5863) H13C(0.741301) H15A(0.2432)
 H15B(0.223701) H15C(0.385) H16A(0.5021) H16B(0.3307) H16C(0.4773)
 H17A(0.277599) H17B(0.146) H17C(0.2087)
 Fixed Y: H2(0.1366) H5(0.154901) H7A(0.1749) H7B(0.084499) H7C(0.149301)
 H8A(0.0005) H8B(-0.063701) H8C(-0.0705) H9A(-0.027101) H9B(-0.026501)
 H9C(0.0665) H11A(0.169901) H11B(0.2662) H11C(0.2042) H12A(0.4091) H12B(0.4135)
 H12C(0.3451) H13A(0.275999) H13B(0.3708) H13C(0.3676) H15A(0.228901)
 H15B(0.3445) H15C(0.2946) H16A(0.426) H16B(0.446699) H16C(0.4084) H17A(0.2877)
 H17B(0.3169) H17C(0.2072)
 Fixed Z: H2(0.939899) H5(0.7908) H7A(0.7026) H7B(0.686399) H7C(0.7699)
 H8A(0.8606) H8B(0.776599) H8C(0.8495) H9A(0.7434) H9B(0.6722) H9C(0.6845)
 H11A(1.108101) H11B(1.1305) H11C(1.0481) H12A(1.0342) H12B(0.9589)
 H12C(0.9506) H13A(1.121101) H13B(1.063101) H13C(1.1369) H15A(0.986099)
 H15B(0.9877) H15C(1.036699) H16A(0.9437) H16B(0.8855) H16C(0.8435)
 H17A(0.777699) H17B(0.8338) H17C(0.8338)
;
_shelx_res_checksum              23226
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'