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_1518500
_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         'C51 H87 As12 Co3'
_chemical_formula_sum            'C51 H87 As12 Co3'
_chemical_formula_weight         1776.03
_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   geom
_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                 112.7520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.9202(3)
_cell_length_b                   15.78990(10)
_cell_length_c                   29.9375(3)
_cell_measurement_reflns_used    15200
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      70.3717
_cell_measurement_theta_min      3.0701
_cell_volume                     12607.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      123.00(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -81.00  -55.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814 -159.0000   95.0000 52

  2 omega  -62.00   30.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   77.0000  -60.0000 184

  3 omega -108.00  -17.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000  -30.0000 182

  4 omega   27.00   73.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -45.0000   30.0000 92

  5 omega   74.00  118.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179 -125.0000 -120.0000 88

  6 omega   26.00   52.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000   60.0000 52

  7 omega   41.00  107.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -94.0000    0.0000 132

  8 omega   23.00   67.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000   90.0000 88

  9 omega   28.00   75.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -45.0000 -180.0000 94

 10 omega   18.00   65.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179    0.0000  -60.0000 94

 11 omega   83.00  157.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179    0.0000  -60.0000 148

 12 omega   28.00   65.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000  -60.0000 74

 13 omega -115.00  -11.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000 -180.0000 208

 14 omega -115.00  -11.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000  -90.0000 208

 15 omega -115.00  -11.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000   90.0000 208

 16 omega   73.00   98.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   45.0000    0.0000 50

 17 omega   73.00  147.50   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   45.0000  120.0000 149
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0558585000
_diffrn_orient_matrix_UB_12      0.0249467000
_diffrn_orient_matrix_UB_13      0.0205638000
_diffrn_orient_matrix_UB_21      -0.0040968000
_diffrn_orient_matrix_UB_22      0.0238318000
_diffrn_orient_matrix_UB_23      -0.0512827000
_diffrn_orient_matrix_UB_31      -0.0141927000
_diffrn_orient_matrix_UB_32      0.0912408000
_diffrn_orient_matrix_UB_33      0.0078313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38088
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.494
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.346
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       plate
_exptl_crystal_F_000             6960
_exptl_crystal_recrystallization_method
'The material was recrystallised from a saturated hexane solution at -25 degree celsius.'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.0352
_exptl_crystal_size_min          0.0066
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         11768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0191P)^2^+1.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10045
_reflns_number_total             11768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03543g1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1518346--1518500.cif.'
_cod_database_code               1518500
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C51 H87 As12 Co3'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C18(H18), C20(H20), C35(H35), C37(H37)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C)
;
_shelx_res_checksum              77842
_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'