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_1518497
_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, C H2 Cl2'
_chemical_formula_sum            'C35 H60 As4 Cl2 Co2'
_chemical_formula_weight         969.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 107.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8930(10)
_cell_length_b                   19.9249(11)
_cell_length_c                   11.6299(5)
_cell_measurement_reflns_used    7048
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.5380
_cell_measurement_theta_min      2.6777
_cell_volume                     3945.5(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_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    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.0(10)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
  1 omega  -56.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0628    0.0000  -30.0000 124

  2 omega  -99.00   11.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0628  -77.0000   30.0000 110
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0410788838
_diffrn_orient_matrix_UB_12      0.0017256743
_diffrn_orient_matrix_UB_13      0.0287187139
_diffrn_orient_matrix_UB_21      -0.0050290598
_diffrn_orient_matrix_UB_22      -0.0146162905
_diffrn_orient_matrix_UB_23      0.0527697952
_diffrn_orient_matrix_UB_31      0.0044534166
_diffrn_orient_matrix_UB_32      -0.0324488885
_diffrn_orient_matrix_UB_33      -0.0223330271
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13850
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.651
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_recrystallization_method
'The material was recrystallised from a saturated DCM solution at -25 degree celsius.'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.679
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0395P)^2^+14.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5548
_reflns_number_total             6515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03543g1.cif
_cod_data_source_block           cg101
_cod_depositor_comments
'Adding full bibliography for 1518346--1518500.cif.'
_cod_database_code               1518497
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.313
_shelx_estimated_absorpt_t_min   0.188
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1S \\sim Cl2 \\sim Cl1: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.005
3. Others
 Fixed Sof: H1SA(0.25) H1SB(0.25) H1SD(0.25) H1SC(0.25) Cl1(0.1) Cl2(0.9)
 Fixed Uiso: H2(0.016) H5(0.017) H7A(0.034) H7B(0.034) H7C(0.034) H8A(0.034)
 H8B(0.034) H8C(0.034) H9A(0.032) H9B(0.032) H9C(0.032) H11A(0.034) H11B(0.034)
 H11C(0.034) H12A(0.039) H12B(0.039) H12C(0.039) H13A(0.036) H13B(0.036)
 H13C(0.036) H15A(0.035) H15B(0.035) H15C(0.035) H16A(0.031) H16B(0.031)
 H16C(0.031) H17A(0.028) H17B(0.028) H17C(0.028)
 Fixed X: H2(0.2436) H5(0.4477) H7A(0.576599) H7B(0.504) H7C(0.5439)
 H8A(0.4157) H8B(0.435399) H8C(0.5037) H9A(0.476799) H9B(0.558101) H9C(0.5328)
 H11A(0.255301) H11B(0.3141) H11C(0.2244) H12A(0.323201) H12B(0.365101)
 H12C(0.3956) H13A(0.194201) H13B(0.1785) H13C(0.228701) H15A(0.327901)
 H15B(0.4161) H15C(0.361201) H16A(0.3696) H16B(0.385) H16C(0.4416) H17A(0.2146)
 H17B(0.2473) H17C(0.232699)
 Fixed Y: H2(0.803) H5(0.727901) H7A(0.9008) H7B(0.915) H7C(0.8422) H8A(0.908)
 H8B(0.9577) H8C(0.933999) H9A(0.7899) H9B(0.828801) H9C(0.771) H11A(1.003301)
 H11B(0.9521) H11C(0.9313) H12A(1.0157) H12B(0.9519) H12C(0.980399)
 H13A(0.9703) H13B(0.8943) H13C(0.9098) H15A(0.6097) H15B(0.6244) H15C(0.5758)
 H16A(0.7222) H16B(0.643001) H16C(0.691801) H17A(0.660901) H17B(0.623201)
 H17C(0.7026)
 Fixed Z: H2(0.167601) H5(0.4135) H7A(0.4832) H7B(0.364901) H7C(0.3868)
 H8A(0.603701) H8B(0.508801) H8C(0.6265) H9A(0.629001) H9B(0.6499) H9C(0.55)
 H11A(0.3842) H11B(0.474199) H11C(0.4108) H12A(0.2291) H12B(0.191901)
 H12C(0.327001) H13A(0.1725) H13B(0.2033) H13C(0.113701) H15A(0.3316)
 H15B(0.333) H15C(0.232599) H16A(0.061201) H16B(0.068901) H16C(0.166901)
 H17A(0.1668) H17B(0.070499) H17C(0.0606)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S(H1SD,H1SC)
;
_shelx_res_checksum              84046
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'