Synthesis of 1,2,3-tripnictolide anions by reaction of group 15 Zintl ions with acetylene. Isolation of [E/3C/2H/2]^-^ (E = P, As) and preliminary reactivity studies
Robert S. P. Turbervill; Jose M. Goicoechea; Chem.Commun. 48 (2012) 6100–; doi:10.1039/c2cc32244g

data_7107855
_publ_contact_author_fax         '+44 1865 272690'
_publ_section_title
;
 Synthesis of 1,2,3-tripnictolide anions by reaction of group 15 Zintl
 ions with acetylene. Isolation of [E/3C/2H/2]^-^ (E = P, As) and
 preliminary reactivity studies
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_journal_name_full               Chem.Commun.
_journal_page_first              6100
_journal_paper_doi               10.1039/c2cc32244g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C18 H36 K N2 O6, C10 H16 As3 Ru'
_chemical_formula_sum            'C28 H52 As3 K N2 O6 Ru'
_chemical_formula_weight         877.65
_chemical_name_systematic
;
[K-(2,2,2-crypt)][(As3C2H2)Ru(Me-allyl)2]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.6810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.73910(10)
_cell_length_b                   17.42280(10)
_cell_length_c                   18.64660(10)
_cell_measurement_reflns_used    53310
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.2207
_cell_measurement_theta_min      3.5502
_cell_volume                     3633.60(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0086
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78137
_diffrn_reflns_theta_full        76.41
_diffrn_reflns_theta_max         76.41
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    7.870
_exptl_absorpt_correction_T_max  0.5717
_exptl_absorpt_correction_T_min  0.2341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+1.1971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                7422
_reflns_number_total             7613
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc32244g.txt
_cod_data_source_block           3
_cod_depositor_comments
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The following automatic conversions were performed:
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Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_original_cell_volume        3633.60(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7107855