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_1518499
_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         'C68 H116 As10 Co4, 4(C H2 Cl2)'
_chemical_formula_sum            'C72 H124 As10 Cl8 Co4'
_chemical_formula_weight         2258.22
_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     direct
_audit_creation_date             2014-10-08
_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                62.971(6)
_cell_angle_beta                 69.895(6)
_cell_angle_gamma                61.292(6)
_cell_formula_units_Z            1
_cell_length_a                   13.7956(8)
_cell_length_b                   14.0892(8)
_cell_length_c                   15.0382(10)
_cell_measurement_temperature    123(2)
_cell_volume                     2254.0(3)
_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(1)
_diffrn_measured_fraction_theta_full 0.772
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.772
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11135
_diffrn_reflns_point_group_measured_fraction_full 0.772
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         62.116
_diffrn_reflns_theta_min         3.343
_exptl_absorpt_coefficient_mu    12.199
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.266
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             1130
_exptl_crystal_recrystallization_method
'The material was recrystallised from a saturated DCM solution at -25 degree celsius.'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6133
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0787
_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/[\s^2^(Fo^2^)+(0.0232P)^2^+59.9927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4426
_reflns_number_total             6133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03543g1.cif
_cod_data_source_block           cg37_2_sq
_cod_depositor_comments
'Adding full bibliography for 1518346--1518500.cif.'
_cod_database_code               1518499
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4B-C35 = Cl4A-C35 = Cl3-C35
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C1 \\sim C18 \\sim C30 \\sim C19 \\sim C26 \\sim C3 \\sim
C24 \\sim C33 \\sim C4 \\sim C6 \\sim C12 \\sim C23 \\sim C29 \\sim C28 \\sim
C27 \\sim C34 \\sim C31 \\sim C32 \\sim C9 \\sim C22 \\sim C7 \\sim C25 \\sim
C11 \\sim C2 \\sim C10 \\sim C5 \\sim C8 \\sim C15 \\sim C13 \\sim C17 \\sim
C14 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Cl4A \\sim C35 \\sim Cl3 \\sim Cl3 \\sim Cl4A \\sim C35 \\sim Cl4B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(H35C)=Sof(H35D)=Sof(Cl4B)=1-FVAR(1)
 Sof(Cl4A)=Sof(H35A)=Sof(H35B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C35(H35C,H35D)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C1(H1), C18(H18), C4(H4)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C33(H33A,H33B,
 H33C), C12(H12A,H12B,H12C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C34(H34A,
 H34B,H34C), C32(H32A,H32B,H32C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C25(H25A,
 H25B,H25C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              94301
_shelx_fab_checksum              265
_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'